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Synthesis Of Phenyl-2-propanone

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Phenyl acetone, Phenyl acetone in india, Phenyl acetone in bulk, best quality Phenyl acetone, Phenyl Acetone (1 Phenyl 2-Propanone), phenylacetone india, CAS NO.:103-79-7 - Phenyl Acetone – p2p, P2P, benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, phenylacetone manufacturers, Manufacturers, Suppliers & Exporters, fine chemicals, MulBerry Chemicals Pvt. Ltd. Phenyl Acetone, 1 Phenyl 2-Propanone, manufacturers, CAS NO.:103-79-7, chemicals manufacturer India, supply, trade, export, manufacturing, fine chemicals, Intermediaries, phenylacetone, phenyl acetone, phenyl acetone chemicals, phenyl-2-propanone, benzyl methyl ketone, methyl benzyl ketone, buy, best quality, manufacturers, suppliers, exporters, mumbai, india, chemical, chemicals, p2p, P2P, chlorohexanone, 6 chlorohexanone, benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, chloro hexanone, dibutyl ether, 1,4 dioxane, 6 methyl quinoline, 2 isobutyl quinoline, 6(8)secondary butyl quinoline, manufacturers, exporters, suppliers, mumbai, india Phenyl Acetone, 1-Phenyl 2-Propanone CAS NO.:103-79-7 - MulBerry Chemicals Pvt. Ltd high quality chemicals Phenyl Acetone, phenylacetone manufacturers, Di-n-butyl Ether, 1, 4 Dioxine, Quinoline and Substituted Quinoline and Grignard reagents etc. We are manufacturers, supplier, exporter of Phenyl Acetone chemicals in India, provides chemicals, p2p,benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, chloro hexanone, dibutyl ether, 1,4 dioxane, 6 methyl quinoline, 2 isobutyl quinoline, 6(8)secondary butyl quinoline, manufacturers, suppliers and exporters in India.phenylacetone, phenyl acetone, phenyl acetone chemicals, phenyl-2-propanone, benzyl methyl ketone, methyl benzyl ketone, buy, best quality, manufacturers, suppliers, exporters, mumbai, india, dialnsearch Phenyl Acetone - Manufacturers, Suppliers and Exporters phenylacetone, (or phenyl-2-propanone, benzyl methyl ketone or methyl benzyl ketone. Often it's referred to as P2P) is an organic compound. It is a clear oil with a refractive index of 1.5168. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. Due to the illicit uses in clandestine chemistry, it was declared a schedule II controlled substance in the United States

Phenylacetone (103-79-7)

SYNTHESIS OF PHENYL-2-PROPANONE

PRODUCT NAME

Phenylacetone

Phenylacetone (known also as phenylpropan-2-one, benzyl methyl ketone, or methyl benzyl ketone), is an organic compound. It is a clear oil with a refractive index of 1.5168. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate, where it is commonly known as P2P. Due to the illicit uses in clandestine chemistry, it was declared a schedule II controlled substance in the United States 11 February 1980. Preparation There are many methods in the scientific literature to prepare phenylacetone, and due to its status as a controlled substance, there is crossover into popular literature such as works by Uncle Fester and Alexander Shulgin. Large amounts of data are available on the Internet relating to the preparation of phenylacetone. A conceptually simple example of phenylacetone organic synthesis is the Friedel-Crafts alkylation of benzene with chloroacetone.

Phenylacetone can also be produced from many other compounds. For example: phenylacetic acid is distilled with lead acetate or calcium acetate to yield phenylacetone. benzaldehyde is reacted with nitroethane yielding phenyl-2-nitropropene, which is reduced, usually in the presence of acid, to phenylacetone. Phenyl acetone is used as an intermediate to produce pesticides and anticoagulants. Active ingredients as anticoagulants include: Brodifacoum Chlorophacinone Coumachlor Difenacoum Diphenadione 2-Pivaloyl-1,3-indandione 2-Isovaleryl-1,3-indandione Warfarin 3,4-Methylenedioxyphenylpropan-2-one (MDP2P) is a chemical compound consisting of a phenylacetone moiety substituted with a methylenedioxy functional group. It is commonly synthesized from either safrole ((which, for comparison, is 3-[3,4-(methylenedioxy)phenyl]-1-propene) or its isomer isosafrole via oxidation using the Wacker oxidation or peroxyacid oxidation methods. MDP2P is a precursor in the chemical synthesis of the methylenedioxyphenethylamine (MDxx) class of compounds, the classic example of which is 3,4-methylenedioxy-N-methylamphetamine (MDMA), and is also an intermediate between the MDxx family and their slightly more distant precursor safrole or isosafrole. On account of its relation to the MDxx chemical class, MDP2P, as well as safrole and isosafrole, are in the United States (U.S.) Drug Enforcement Administration (DEA) List I of Chemicals of the Controlled Substances Act (CSA) via the Chemical Diversion and Trafficking Act (CDTA).

Phenyl Acetone (1 Phenyl 2-Propanone). catalyzed by Mn3+ Oxythallation of alpha-methylstyrene Wittig reaction of Benzaldehyde Cu(I)-catalyzed Arylation of Potassium Acetylacetonate Pd-catalyzed Arylation of Isopropenyl Acetate Alkylation of Benzyl cyanide with Trimethylaluminium P2P from Phenylacetaldehyde and Dimethyl Cadmium P2P from Phenylacetyl Chloride and Dimethyl Cadmium P2P via Grignard Addition to Acetic Anhydride P2P via Grignard Addition to Benzyl Cyanide References ----------------------------------------------------------------------------------------\ Introduction Aside from the often amateurish reduction of (pseudo)ephedrine to methamphetamine. phenylacetone.:103-79-7 .phenylacetone. but there has always sprung up new methods of performing the feat of making this compound. 6 methyl quinoline. phenyl acetone manufacturers. p2p. exporters. the most popular precursor to amphetamine and methamphetamine is phenyl-2-propanone (also called P2P. dialnsearch Phenyl Acetone Manufacturers. Often it's referred to as P2P) is an organic compound. exporter of Phenyl Acetone chemicals in India. CAS NO. 2 isobutyl quinoline.Phenyl acetone. phenyl 2 propanone. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. ranging from simple one-step methods to elaborate multi-step variants. provides chemicals. Phenyl acetone in india. Many of the earliest routes to the compound has been more or less abandoned due to restrictions on the pre-precursors used to make it. trade.4 dioxane. phenyl acetone suppliers.5168. phenyl acetone chemicals. phenylacetone india.:103-79-7. best quality Phenyl acetone. Appearance: Clear oil. Here is a collection of some of the possible methods of synthesizing phenyl-2-propanone.4-methylenedioxyphenyl-2-propanone) by using starting materials with the desirable aromatic substituents. mumbai. Welcome to the world of P2P. 2 isobutyl quinoline. dibutyl ether. dibutyl ether. Phenyl Acetone. supplier. chlorohexanone. 6 chlorohexanone. methyl benzyl ketone. Suppliers and Exporters phenylacetone. phenyl acetone manufacturers. india. exporters. use Phenyl acetone.benzyl methyl ketone. buy. 1 Phenyl 2-Propanone.:103-79-7 . fine chemicals. phenyl acetone. There is an astounding array of synthetic routes to this compound. fine chemicals. phenyl acetone exporters. both due to the relative simple structure of the compound. phenyl acetone suppliers. Benzyl Methyl Ketone or Phenylacetone). Intermediaries. chloro hexanone. benzyl methyl ketone. Ltd high quality chemicals Phenyl Acetone. benzyl methyl ketone or methyl benzyl ketone.19 g/mol Density: 1. 1. It is a clear oil with a refractive index of 1. phenyl acetone suppliers.Phenyl Acetone – p2p. 4 Dioxine. suppliers and exporters in India. chemicals manufacturer India. benzyl methyl ketone. MulBerry Chemicals Pvt. BMK. phenyl-2-propanone. benzyl methyl ketone. 6 methyl quinoline. benzyl methyl ketone. Many of the syntheses can also be tweaked to produce substituted phenyl-2-propanones. use Phenyl acetone. Phenyl acetone in india. 6(8)secondary butyl quinoline. 1. phenyl 2 propanone. such as the ever popular MDMA precursor MDP2P (3. best quality Phenyl acetone Phenyl acetone. 1. p2p. Due to the illicit uses in clandestine chemistry. and also because of its popularity. phenyl-2-propanone. supply. and from the very easy to the very complicated. phenyl acetone.5168 . manufacturing. manufacturers. best quality. chemical. export. suppliers. flowery odor Boiling Point: 214-216°C/760mmHg. Suppliers & Exporters. suppliers. P2P. chloro hexanone. 6(8)secondary butyl quinoline. We are manufacturers. phenyl 2 propanone. phenyl acetone chemicals. phenylacetone manufacturers. manufacturers. manufacturers. manufacturers.MulBerry Chemicals Pvt. Ltd. phenylacetone manufacturers. methyl benzyl ketone. mumbai. Phenyl acetone in bulk. 86-87°C/6mmHg Melting Point: -15°C Molecular Weight: 134.0057 g/ml (20°C) Refractive Index: 1. CAS NO. exporters. mumbai. india. phenyl acetone exporters. chemicals.4 dioxane. 1-Phenyl 2-Propanone CAS NO. Di-n-butyl Ether. Quinoline and Substituted Quinoline and Grignard reagents etc. phenyl acetone exporters. P2P. buy. (or phenyl-2-propanone. best quality. Manufacturers. suppliers. india Phenyl Acetone. it was declared a schedule II controlled substance in the United States Synthesis of Phenyl-2-Propanone (P2P) Table of Contents Table of Contents Introduction P2P from Benzyl Cyanide P2P from Phenylacetic Acid Friedel-Crafts Alkylation of Benzene with 2-Nitropropane Reduction of Phenyl-2-Nitropropene Friedel-Crafts Alkylation of Benzene with Chloroacetone Hydrolysis of Ephedrine Derivatives Electrochemical Coupling of Benzyl Chloride and Acetic Anhydride Nickel-mediated Coupling of Benzyl Chloride and Acetyl Chloride Semipinacol Rearrangement of Phenyl-2-Propanal P2P from Bromobenzene/Acetone Enolate Radical Alkylation of Benzene with Acetone. phenyl acetone manufacturers. manufacturers.

and discarded. Phenyl-2-Propanone2 350 ml of concentrated sulfuric acid is placed in a 3000ml flask and cooled to -10°C. it weighs 125-150g (77-86% of the theoretical amount). washed with ether. The ether is removed from the filtrates. The fraction boiling at 110-112°C at 24 mmHg is collected.3 moles of dry product) is added slowly. The next morning the mixture is stirred with a wooden rod to break lumps.2-1. The precipitate separated by suction filtration and washed four times on the funnel with 250 ml portions of water. The mixture is thoroughly shaken. while the temperature is kept below 10°C. the solution cooled to 0°C. and the flask placed on a vigorously boiling water bath and heated for two hours. The filter cake is practically colorless and corresponds 250-275g of dry sodium salt. The sodium salt still wet with ether is dissolved in 1. The sodium sulfate is collected on a filter. The sodium salt is collected on a 6 inch Buchner funnel and washed four times on the funnel with 250 ml portions of ether. cooled in a freezing mixture to 10°C. and the solution heated on the steam bath for two hours before standing overnight. To the hot solution added a mixture of 234g (2 moles) of pure benzyl cyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P2O5 for 30min followed by distillation).Phenyl-2-Propanone from Benzyl Cyanide alpha-Phenylacetoacetonitrile1 A solution of sodium ethoxide is prepared from 60 g. after cooling. with occasional shaking. A somewhat higher yield has been obtained by a different variation of this synthesis. is separated and the acid layer extracted with 600ml of ether. the ether combined with the oil and dried over 20g of anhydrous sodium sulfate. The combined filtrates are placed in the freezing mixture until they can be worked up as indicated below. 1750ml of water added rapidly.3 liters of distilled water at room temperature. The oil and ether layers are washed successively with 100ml of water. and kept at this temperature for two hours. The moist cake weighing about 300g corresponds to 188-206g (59-64%) of dry colorless alphaphenylacetoacetonitrile. the temp being kept below 20°C (If pure dry alpha-phenylacetoacetonitrile is used. (2. originating from Russia. . The ketone forms a layer and. The solution is cooled to 0°C. and the nitrile precipitated by adding slowly. or 69-76% of the calculated mount. with shaking.6 mol) clean sodium and 700 ml of absolute alcohol (dried over calcium oxide or sodium) in a 2000 ml round-bottomed flask equipped with a reflux condenser. After all is added the flask is warmed on the steam bath until solution is complete and then for five minutes longer. with vigorous shaking. and the residue distilled from a modified Claisen flask with a 25 cm fractionating side arm. half its weight of water should be added to the sulfuric acid or charring will take place on the steam bath). mp 87-89°C. The total first crop of moist alpha-phenylacetoacetonitrile obtained according to the procedure above (corresponding to 188-206g or 1. the condenser closed with a calcium chloride tube. 90 ml of glacial acetic acid.

026 mole (3. The reflux setup is rearranged for distillation and excess solvent is removed (acetic acid and acetic anhydride.1 mol).6 g. Formation of the ketone is controlled by mixing an aliquot of the reaction mixture with excess of water and ammonium hydroxide until weakly alkaline – upon heating to boiling the oily layer must not disappear. A vivid reaction took place. which requires liberal application of heat. CaCl2). The Lead(II)Acetate can be substituted with Calcium(II)Acetate. 500 ml acetic anhydride and acetic acid are distilled off. and the crude phenyl-2propanone is vacuum distilled at 25 mmHg. Sodium Acetate Method (alternative)3b 50 g phenylacetic acid. a reflux condenser protected by a sodium hydroxide drying tube and magnetic stirring was placed 0. just to create sufficient bubbles for stirring the solution during the experiment. The yield about 30ml (70%). After 2-3 minutes the gas stream was slowed down. Lead Acetate Method6 Place 1000g phenylacetic acid and 3000g anhydrous (or trihydrate) lead acetate in a distillation apparatus and heat. After separation of layers upper layer is removed and lower layer is three times decanted with water. 0. and next phenyl-2-propanone in this destructive distillation. If necessary. Methyllithium addition to Phenylacetic Acid27 In a 100ml rb flask equipped with a side tube for a gas inlet capillary. Phenyl-2-Propanone Ketoxime was obtained in 88-90% yield.1 mol) anhydrous cupric sulphate is introduced 2000 ml anhydrous acetic anhydride in 4000 ml flask. and the air was then expelled with a rapid stream of dry nitrogen. If the ratio is too small. it is important that acetic anhydride is present in the reaction mixture in a large molar excess over the phenylacetic acid. the solution was then refluxed for 10-30 minutes to complete the reaction. Yield 70-90 g (52-67%). bp 30-64°C/0. the ether refluxed. Potassium Acetate/Copper Sulfate3c To a mixture of 136 g (1. separated.5 g (56%) phenyl-2-propanone. To the residue there is added 400ml water and the mixture is extracted with 3x100mL dichloromethane (or chloroform). which was distilled at 154-156°C/30mmHg. which on fractional vacuum distillation gave 7. making the synthesis more environmentally friendly. When all air had been expelled 0. . the phenylacetone will condense with itself to form useless Dibenzyl Ketone. the rest is mixed with 1000 ml water after cooling down. Remaining acetic acid and acetic anhydride is then removed. 70 g sodium or potassium acetate. The organic layer is separated and redistilled to give pure phenyl-2-propanone. The excess of methyllithium was thus destroyed and lithium hydroxide was formed from the intermediate dilithium salt. Sodium Acetate Method (alternative)3b The Phenylacetic Acid (PAA). The distillate will separate into two layers. Heating of the reaction mixture to 145-150°C on an oil bath provides sufficiently energetic evolution of carbon dioxide. the crude product is extracted with 2x250ml dichloromethane and the pooled organic layers are washed with cold diluted sodium hydroxide solution (any formed P2P enol ester must be hydrolyzed) until no more acids are present in the organic layer.5 g) of phenylacetic acid dissolved in 50 ml of ether. A second distillation gives 50-55% yield of product boiling at 210-215°C at atmospherical pressure. First an amount of water will distill. bp 105°C/10 mmHg or 216°C at atmospherical pressure. The solution is dried over Na2SO4 and the dichloromethane is distilled off under ordinary pressure (and is saved for reuse) the rest of the volatiles are evaporated in vacuo. and distilled. A considerable improvement to this method has been made by Xtaldoc on a large scale. After the solution had reached room temperature.0 mol) phenylacetic acid. purify and reuse). Removal of the solvent left a residue witging 12g. and 16 g (0. Acetic Anhydride (AA) and Sodium Acetate (NaOAc) is put in to a large round-bottomed flask equipped with a reflux condenser fitted with a drying tube. After the addition of all the methyllithium the precipitate partly dissolved and a weakly opalescent solution was obtained. The mixture is refluxed 24 h. Pyridine Method5 A mixture of phenylacetic acid (13. After cooling 500 ml of solvent (CCl4. After removal of the solvent the residue was taken up in toluene and washed with 10% sodium hydroxide.1mmHg. bp 120-140°C. pure product is collected at 100°C/15mmHg. The solvent is stripped off under vacuum and by vacuum distilling at 125-135°C/30-32 mmHg the crude product is obtained. dried (Na2SO4. 25 g anhydrous sodium acetate and 850 ml acetic anhydride are refluxed with stirring under moisture protection for 40 h. CHCl3. The solvent is distilled off and fractionation column is placed on the top of the flask. CH2Cl2) is added and the mixture is poured to a flask containing 2000 ml icewater. acetic anhydride (50 ml) and pyridine (50 ml) was refluxed six hours (in the beginning carbon dioxide evolution was vigorous.Phenyl-2-Propanone from Phenylacetic Acid In this reaction.055 mole of an ethereal solution of methyllithium was added through the condenser. water was slowly added. and a white precipitate was formed (lithium salt of the acid).

the aqueous phase extracted with CH2Cl2. The combined extracts was washed with 2x150 ml H2O and dried over MgSO4. recrystallized from methanol. When the generation of heat had subsided. and was extracted with 3x100 ml CH2Cl2. When the pH of the solution turned acid. as a colorless oil. and the pooled organic extracts washed with 1 M Na2CO3 solution and dried over MgSO4. 39g) at room temperature. During the addition of H2O2/K2CO3 a white. Titanium tetrachloride (0. and the residue distilled under vacuum to give phenyl-2-propanone in 75% yield. 0. neutralized with powdered NaHCO3 and saturated with NaCl. Reduction with Iron Powder13 If phenyl-2-nitropropene is reduced by iron powder in an acidic medium (such as acetic acid or aqueous hydrochloric acid) the nitroalkene is reduced to the oxime. The organic phase was dried over MgSO4. after which the precipitate will be much looser and no match for any mag-stirrer. Then. The solution was extracted with 3x100ml CH2Cl2. water (150 ml) was added and the resultant heterogenous mixture was stirred at reflux for 2h. Triflic Acid Method14 A solution of 2-nitropropene (300 mg) in benzene (30 equivalents) was added to a well-stirred solution of CF3SO3H (10 equivalents with respect to 2-nitropropene) and benzene with the co-solvent of methylene chloride cooled to -40°C in a dry ice-acetone bath. followed by hydrolysis of the nitro group with hydrogen peroxide and potassium carbonate. which is then hydrolyzed by the acid into the desired phenyl-2propanone.6g (0. After being stirred for 60 min (or when the starting material completely disappears on TLC). At the end of this period. the solution is slowly acidified with 2M HCl with good stirring.3g (0. with good stirring. The solution was extracted with CH2Cl2. 100 ml of 30% H2O2 was then added. a variety of the Nef reaction. and the ethereal layer washed three times with half its volume of water. filtered and the ether driven off. and the mixture was refluxed on low heat for 1. 61 mmol) was dissolved in 75 ml HOAc and slowly dripped into a refluxing slurry of Fe powder (32 g. but the acidity was confirmed with pH paper.4 dinitrophenylhydrazone derivative. as the side chain tends to be oxidized when electron-donating substituents are present on the ring. phenyl-2-nitropropene is reduced to phenyl-2-nitropropane with NaBH4 in methanol. 16. The mixture turned brownish and foamy. The reaction mixture was poured into 2000ml water. The organic phase was separated.The alkaline water layer. without isolation of the intermediate. and the residue was flash chromatographed (on SiO2. After distillation of said oil at aspirator vacuum.1 mol. so the mass can be stirred with a glass rod now and then during the first two hours. was removed in a separatory funnel. and the pooled organic extracts washed with 100ml 2M NaOH and 200ml H2O. Phenyl-2-Propanone from Phenyl-2-Nitropropene8 Sodium Borohydride/Nef Reaction In this preparation. had mp 152. and chilled to 0°C with an ice/salt bath.5°C. Reduction with Chromous Chloride18 Another method for reducing phenyl-2-nitropropene to phenyl-2-propanone in 80% yield is to use Chromium(II)chloride as the reducing agent.57 mol) in 140 ml HOAc. 19g) was then added dropwise into the mixture with stirring at the same temperature. 70% of theory). together with 30 grams of anhydrous potassium carbonate. usually pure enough for most purposes. dried over Na2SO4. which can be a bit too thick for a weak magnetic stirrer to handle. After being warmed to ambient temperature (10-15 min). Evaporation of the solvent followed by vacuum distillation (bp 100-101°C at 14mmHg) afforded Phenyl-2-propanone (ca 9g. Phenyl-2-propanone by nitroalkylation of benzene Titanium Tetrachloride Method7 To a stirred solution of 2-nitropropene (0. 8.5 h. sticky precipitate forms.bath was removed and the solution was stirred at room temperature for two hours. first at ordinary pressure and then at aspirator vacuum to give 2. The reaction mixture was immediately (after 1 minute) poured into large excess dry methanol (100 mL) cooled to -78°C with vigorous stirring. and the solvent removed under vacuum to give a clear yellow oil. and the temperature was not allowed to to rise above 15°C. The solvent was distilled off. the yield was around 60-70% of phenyl-2propanone (P2P) as a light yellow oil.1 mole) phenyl-2-nitropropene was dissolved in 200ml methanol in a 250ml Erlenmeyer flask situated on a magnetic stirrer. which contained the lithium salt of unreacted acid. All of the precipitate was also be gone at this point. the flask was once again placed in an ice/salt bath and the solution was allowed to cool to 0°C again. the yellow solution was diluted with water (150 mL). About 300 ml of acid is needed. and the solution was left to stir for 18-24 hours at room temp.5 mol. the ice/salt. The ether solution was then dried over magnesium sulphate.5-153. eluting with CH2Cl2:n-hexane 12:7) to give pure phenyl-2-propanone.7g) in dry CH2Cl2 (300ml) was added benzene (0. the color became significantly more yellow. Phenyl-2-nitropropene (10 g.65g (76%) of phenylacetone. 392 mg (85%).1 mol. care being taken for the evolution of heat and CO2. 7. . The next day. The 2. The preparation is a one-pot synthesis. filtered with suction. and concentrated. This synthesis is not suitable for ringsubstituted phenyl-2-nitropropenes.2 mole) of NaBH4 was added a little at the time.

Nine grams of liquid boiling below 123°C/20-22mmHg was obtained.2 faradays per mole of benzyl chloride). and a mixture of appropriate reagents in glyme (10 mL) was then added to the nickel. 21-30 mmol). During the reduction the surface of lithium became pink. 130g (82%) of phenyl-2-propanone is isolated in a purity of 99. a reflux water condenser and a small addition funnel. which then can be hydrolyzed into phenyl-2propanone and an amine salt. filtering.5 g (32%). The flask was evacuated and filled with argon two or three times. After refluxing for 5 hours. When no more hydrogen chloride was evolved. The mixture was stirred and heated to refluxing on a steam bath and 13.16 mol) Ephedrine or Pseudoephedrine freebase was dissolved at a temperature of 50-100°C. Electrosynthesis of P2P from Benzyl Chloride4 Synthesis of phenyl-2-propanone from benzyl chloride (79 mmol) and acetic anhydride (686 mmol) by electrolysis of the reaction mixture. for details. which spontaneously can rearrange to the isomeric imine (Schiff Base). As all the steps are reversible processes. After the lithium metal was consumed completely. Metallic Nickel-Mediated Synthesis of P2P from Benzyl Chloride and Acetyl Chloride28. and phenyl-2-propanone.0 equiv.3 mmol) were placed in the flask through the side neck. The use of a glovebox or bag is not required if contact of the lithium with air is kept to a minimum. lithium (2. Ephedrine derivatives that can be used in this procedure include Ephedrine.1 equiv. the reaction mixture was decomposed by slowly adding water through the condenser. metallic nickel which had adhered to the walls of the flask was scraped off with the stirrer and a magnet. Many other metal salts can be used instead of the zinc chloride. The benzene layer was separated and the aqueous layer extracted with four 25 ml portions of benzene. is isolated by toluene extraction of the distillate. Norephedrine and Norpseudoephedrine (Phenylpropanolamine). see the translation of the original patents.9 g (0. 9-13 mmol). both in free form and in the form of its enol acetate. the ether dried over anhydrous MgSO4 and the ether distilled on a steam bath. and the remaining viscous oil was distilled under reduced pressure. Nickel halide (1. 6 mmol). they are dehydrated to the enamine. All of the benzene solutions were combined and filtered. The the crude phenyl-2-propanone.8%. DMF as the solvent and a tetrabutylammonium tosylate electrolyte gives a 73% yield of phenyl-2-propanone after hydrolysis of the resulting enol ester. Yield 6.Phenyl-2-Propanone from Chloroacetone9 41 grams (0. using a lead cathode and a carbon anode. Phenyl-2Propanone was recovered from the distillate by making the bisulfite addition product. Phenyl-2-propanone from Ephedrine Derivatives10 When ephedrine and related compounds are heated in strong aqueous acid. are present in the solution. stirring during the addition. 20 ml of water and 20 ml of concentrated hydrochloric acid was added. After cooling to room temperature. the stirring was stopped.3 equiv. glyme (25-30 mL) was added through the septum with a syringe.31 mole) of anhydrous aluminum chloride and 100 ml of anhydrous benzene (free from thiophene) were put in a 500ml three-necked flask which was equipped with a mercury-sealed stirrer. Then. a rubber septum. and a condenser topped with argon inlet and outlet to oil pump. The top of the condenser was connected to a sulfuric acid trap and this trap was connected to a gas absorption bottle. the remaining benzyl chloride. Approximately 10g of high-boiling material was left in the distilling flask.15 mole) of chloroacetone was allowed drop in slowly during a period of 30 minutes. After distillation through a short vigreaux column. and weighed. The anode is made of magnesium or aluminium. and during 2. bp 108-114°C/20-22mmHg. The glass tube was evacuated to evaporate the hexane. which is free from propiophenone. The distillate was extracted with ether. The benzene was distilled off.5-3 hours the phenylacetone is steam distilled from the reaction mixture. and the reaction mixture was heated further to 145-150°C. filled with argon. and 192g (1. decomposing the addition product with sodium carbonate solution. the solution was practically black. Lithium metal was cut under mineral oil. At 125°C steam is passed through the solution to facilitate mixing of the contents. After the electrolysis using a current of 1A at a temperature of 0°C (2. the reaction equilibrium is driven towards the desired product by continuously removing the formed phenyl-2-propanone by the aid of steam distillation. The phenyl-2Propanone was distilled under reduced pressure. The nickel precipitated as a bulky black powder in a clear colorless solution after standing. Another procedure33. One piece of lithium with a shining metal surface was rinsed in hexane and transferred into a glass tube with a stopcock and a rubber septum which had been filled with argon. The septum on the side neck was replaced with an addition funnel.9-1. the toluene which is a byproduct of the reduction of benzyl chloride. and naphthalene (0. At 145°C the stream of steam is increased.29 Preparation of Metallic Nickel A 50-mL two-neck flask was equipped with a magnetic stirrer. 0. After the DMF has been evaporated off and the residue has been hydrolysed with hot dilute HCl. . 1025g 75% sulfuric acid was mixed with 1g ZnCl2. and the mixture was stirred for 12 h. Pseudoephedrine. the cathode of nickel. the solvent is DMF (110g) and the supporting electrolyte is tetrabutylammonium fluoroborate (2 g. phenyl-2-propanone is isolated by extraction with ether in 64% yield. and steam distilled as long as any oil distilled over.

and is not disastrous for your health or the environment. 2-Phenyl-propanal (hydratropic aldehyde) is an unwatched industrial chemical which is used in the perfume industry. Method B 9 g of 2-phenylpropanal is slowly added with good stirring during 35 minutes to 40ml concentrated sulfuric acid. the mixture is allowed to stand at the same temperature for another 15 minutes.152 g. When the ice has melted. poured into a separatory funnel containing hydrochloric acid solution (37%. IR (neat) 1710 cm-1 (C=O). 2-phenylpropanal can also be made from alpha-methylstyrene. alpha-methyl benzeneacetaldehyde and alpha-methyl phenylacetaldehyde. but which will oxidize the aldehyde to 2-phenylpropionic acid.0 g. and naphthalene (0. the organics are extracted from the water phase by 3x50ml diethyl ether.97 mmol). There are other ways of performing this rearrangement. 222°C/760mmHg. Additional heating was continued for 15 min. Phenyl-2-Propanone by Rearrangement of 2-Phenylpropanal11 2-Phenylpropanal can be rearranged with either mercuric chloride (HgCl2) or sulfuric acid (H2SO4) to form the isomeric phenyl-2-Propanone (P2P).6g (62%) of phenyl-2-propanone. during which time a precipitate forms.5h at 100°C in a boiling water bath. the rest consisted of unchanged aldehyde. The crude oil was purified by silica gel chromatography. the pooled organic phases dried over MgSO4. enough to poison a medium-sized lake if released into the environment. 21. but the size of the column that would have to be used makes that option impractical. When 0. and synonyms for it include Hydratropic aldehyde. The distillate is extracted with ether. The CAS number for 2-phenyl-propanal is [93-53-8].122 g. 2Phenylpropionaldehyde. Even if the method below which uses mercuric chloride is higher yielding than the one using cold sulfuric acid. A mixture of benzyl chloride (1. Water is added. After all the 2-phenylpropanal has been added. 100 mL). and the aqueous phase was extracted with additional chloroform. as it is much cheaper to use. The oily residue is then vacuum distilled with a fractionating column to collect the phenyl-2-propanone in a yield of 80% or more. and extracted with chloroform twice. followed by condensation of the vapors and redistilling the P2P12. 1 eq. and if you happen to ingest it yourself. and the solution is steam-distilled (during which operation the precipitate redissolves). Fractional distillation could theoretically be used to separate them. It is not possible to effectively separate 2-phenylpropanal (bp 222°C/760mmHg) from phenyl-2-propanone (bp 214°C/760mmHg) through simple distillation and certainly not via vacuum distillation as the boiling points are too close. 60g of mercuric chloride contains 45 grams of mercury. the solvent removed under vacuum and the residue vacuum distilled to give pure P2P. . it will accumulate in your body. The P2P stays in the organic layer. Boiling point 92-94°C/12mmHg. which is then dried over MgSO4.95 mmol). Cumenealdehyde. The combined extracts were dried over anhydrous sodium sulfate and concentrated.9 mmol). lithium (0.1 equivalents of HgCl2 was used. and the solvent is evaporated. bp 92-101°C at 14mmHg. the ether distilled off and finally the residue is vacuum distilled (bp 91-96°C at 11 mmHg) to give 5. The chloroform solution was washed with water.65 g. It was eluted with hexane followed by chloroform to give phenyl-2-propanone (0. only 10% phenyl-2-propanone was formed. 8.Reaction of Benzyl Chloride with Acetyl Chloride in the Presence of Metallic Nickel Metallic nickel in glyme (25 mL). The acid can then be separated from the ketone by dissolving the mixture in a non-polar solvent and washing the solution with dilute sodium hydroxide. bp 95-96°C (11 mmHg). 7.9 mmol) and acetyl chloride (0. was heated to reflux. 2-phenylpropanal is isomerized to phenyl-2-propanone in up to 87% yield by passing its vapor over an iron zeolite catalyst bed at 500°C. and the red-brown reaction mixture was cooled to room temperature.) and 450ml 75% ethanol in a pressure-safe sealed glass container for 4. 68%). and then the mixture is poured onto crushed ice (100-150g is probably a suitable amount).72 g. prepared from nickel iodide (2. A good idea for separating a mixture of the two is to oxidize the mixture with a mild oxidant which won't affect the P2P. Method A 30g of 2-phenylpropanal is heated together with a mixture of 60g mercuric chloride (HgCl2. dried. I would definitely reccommend the one with sulfuric acid.3 mmol) in glyme (10 mL) was added dropwise for 30 min. while the temperature of the reaction mixture is kept at -16°C. 0.

and to give phenyl-2-propanone in 40% yield (1. After standing for 40 h the mixture was filtered and washed with ether giving a white solid (112g.Phenyl-2-Propanone from Acetone Enolate If acetone is reacted with a strong base. and the residue vacuum distilled to give 10. . which is able to deprotonate one of the relatively acidic alpha protons of the ketone. lithium diisopropylamide and several alkoxides. a compound easily prepared from potassium permanganate. The reaction mixture was partitioned between 400ml ether and 250ml water. The colorless crystals of Thallium(III)Nitrate trihydrate are filtered.29 mol) and alpha-chloroethyl methyl ether16 (28. Phenyl-2-Propanone by Oxythallation of alpha-methylstyrene with Thallium(III)Nitrate23 Warning: Thallium salts are exceedingly toxic. The reaction relies upon the special oxidative powers of manganese(III)acetate. to give pure phenyl-2-propanone enol methyl ether). If this enolate of acetone is allowed to react with a halobenzene (preferably iodobenzene. The yields in the reactions range between 50 and 98%. which is the limiting reagent in this reaction. 88%) consisting of the crude phosphonium salt containing one molar equivalient of benzene crystallization. and requires high dilution of the reactants. alpha-Methylstyrene can also be treated with Bromine and Sulfuric Acid to yield P2P.4g.9g Phenyl-2-Propanone (81% yield). washed with a little methanol.4g. The yield is relatively low. The mixture was allowed to warm to room temp over 1h and was then directly distilled. There are no theoretical obstacles at all to why it would not work in the production of phenyl-2propanone. The phosphonium salt (33 mmol) was suspended in 40 mL of glyme at -40°C under nitrogen. as can be seen in the comprehensive Manganese(III)acetate catalyzed aromatic acetonylation document on this site. and after standing for 15 minutes. and there is an immediate precipitation of Thallium(I)Nitrate. The ylid resulting from treatment of the phosphonium salt with base was found to be very unstable at room tempature. but this can be improved. and the filtrate is shaken for 5 min with 1M H2SO4 to hydrolyze the formed Phenyl-2-Propanone dimethyl acetal. benzene (150ml).4g. but bromobenzene should also work) in DMSO under rigidly anhydrous conditions. The salt is readily soluble in methanol and dilute mineral acids. washed with a little dilute nitric acid and dried in vacuo over phsphorus pentoxide. This salt is slightly hygroscopic on exposure in air but can be stored indefinitely in a sealed container. read Drone #342's Enolate Phenylacetone Synthesis FAQ 1. For a more in-depth discussion of this synthesis. helium or nitrogen) until the dark brown color of manganese(III)acetate changed to the pale pink of manganese(II)acetate (about 90 min). but other ketone enolates. the characteristic red color dissappearing within a few seconds.34g) based on the reacted manganese(III)acetate. At this point a solution of benzaldehyde (30 mmol) in 5 mL of glyme was added over five minutes. oxygen or UV light. 100 mmol) in 100ml methanol is added to a solution of alpha-methylstyrene (11. The ether was then dried over anhydrous Na2SO4 (or MgSO4). the two species will combine to form phenyl. A mixture of Manganese(III)acetate dihydrate (13. Thallium(III)Nitrate 50g Thallium(III)Oxide (Tl2O3) is dissolved in 150ml warm. The solution is extracted with ether. Phenyl-2-Propanone from Benzaldehyde and a Phosphonium Ylide (Wittig reaction)15 The phosphonium salt was prepared by dissolving triphenyl phosphine (76. There has been no known actual attempts at this synthesis using the enolate of acetone and a halobenzene in DMSO (but it has been done in liquid ammonia).0 Free-Radical alkylation of Benzene with Acetone Catalyzed by Manganese(III)Acetate17 Phenyl-2-Propanone can be made in a single step by a free-radical reaction between benzene and acetone. Such strong bases include sodium amide. 50 mmol).82g. acetone (150ml) and glacial acetic acid (250ml) was refluxed under an inert atmosphere (argon. The reaction can be catalyzed by iron salts.2-propanone. dried over MgSO4 and the solvent distilled off. for example potassium tert-butoxide. The ether layer was separated and washed with 250ml water and with 2x250ml 5% Na2CO3 to remove any remaining acetic acid. 100mmol) in 50ml methanol at room temperature with stirring. the solvent evaporated and the residue fractionately distilled to recover unreacted benzene. Potassium tert-butoxide (33 mmol) in 15 mL of glyme was added with stirring over 5 minutes. the preparation and reaction of this ylid was best carried out at -40°C. the precipitate is filtered off. Thallium(III)Nitrate (mol wt 390) is stable indefinitely if stored in tightly sealed bottles. acetone enolate is formed in quantitative yield.30 mol) in 125 mL benzene. such as pinacolone has been extensively studied in this medium. concentrated nitric acid and cooling the pale yellow solution to 0°C. and the reaction is also applicable for other substituted benzenes. and may be lethal upon ingestion! Handle with gloves only! A solution of Thallium(III)Nitrate (39g. 0. Accordingly. 0.

funnel.75g of crude phenyl-2-propanone as an oil. 90 mmol) and dichloro-bis-(tri-otolylphosphine)palladium (0. keep it covered and protected from air. Attach 125ml sep. the flask will have a tannish brown solid mass inside. under nitrogen. sodium bicarbonate. dried over magnesium sulphate and concentrated in vacuo to leave a dark brown oil. add 31. The residue was chromatographed on silica gel. 100 at 13 mm. anhydrous ether. Separate. of halide ether solution to enter flask. After being cooled to 0°C. of chipped ice. Be prepared to stop and cool with ice water bath if needed. anhydrous diethyl ether to sep. Add dropwise the aldehyde/ether solution to the dimethyl cadmium swirling occasionally to break up the clumps. Aldrich).2 grams of anhydrous cadmium chloride in small portions through side neck restoppering after each addition. Neutralize with sat. Distill under reduced pressure to strip off excess ether. which can be purified by vacuum distillation or column chromatography. 3-neck rb. add halide dropwise as quickly as the reflux column can handle. Ethyl acetate was added and the mixture was vigorously stirred for one hour. Yield 50-55 ml. The solution was heated to boiling and the solvent was then evaporated to give relatively pure phenyl-2-propanone in 88% overall yield. add 31. For this preparation it also needs to be as dry as possible. ~85% of P2P. Phenyl-2-Propanone To a clean dry sep. brine and dried over MgSO4. DRY FLASK attach a reflux condenser. When reflux has subsided do not heat. replace stopper. Phenyl-2-Propanone by Heck Arylation22 To a stirred solution of bromobenzene (60 mmol). The mixture was stirred and heated at 100°C for 24 hr. was added tributyltin methoxide (25. freshly distilled phenylacetaldehyde (Note 1) and 50 ml. 10 ml. beaker containing 100 ml. After all the Cadmium chloride has been added.3 ml. Be prepared to stop addition and cool if needed. 200 mmol) in DMF (1 liter) was added cuprous iodide (32. When all the halide has been added and the reaction is no longer refluxing. to afford the phenyl-2-propanone in 67% yield. Add 12.4g. . Phenyl-2-Propanone from Phenylacetaldehyde and Dimethyl cadmium Dimethyl Cadmium 2 MeMgI + CdCl2 => Me2Cd + 2 MgICl To 500 ml. 834 mmol. This is the dimethyl cadmium.9 ml.5 grams Magnesium turnings to flask. Note 1: The phenylacetaldehyde will polymerise on standing.67 mmol) in dry toluene (30 ml). Add 60 ml. which after purification gave phenyl-2propanone in 65% yield. the solution was poured over crushed ice and made acidic with 6M HCl.47g. Allow aprox. HCl and 100 cc. methyl iodide either freshly prepared or dried overnight with calcium chloride. 0. Test with bisulfite any product not forming addition is phenyl-2-propanol (very small amount) can be saved for later oxidation. If cloudiness does not become apparent in 1 or 2 min stop. and extract water layer with 2x50 ml portions of technical grade ether. Add 75 ml anhydrous ether to flask.4 g. funnel. Hydrolyse addition product and distill if desired. The organic layer was washed with aqueous NaHCO3. distilled water 10 ml conc. Do not add more! Take a glass rod about 12 inches in length and score with a 3 corner file 2 inches from one end using pliers and a rag to protect your hands break away the 2 inch piece. 90 mmol. Notes: Avoid breathing the cadmium chloride dust (it needs to be finely ground after drying) avoid contact with the methyl iodide or ether solution of methyl iodide avoid breathing any vapours of the metal conversion reaction (it smells like garlic if you must know). The combined extracts were washed with water. cooled and the solvent evaporated in vacuo. Phenyl-2-Propanone from Benzyl cyanide and Trimethylaluminum25 Trimethylaluminium (30ml of a 2M solution in toluene) was added to a solution of benzyl cyanide (2. aq. Proceed immediately to next part if at all possible. Quickly pour into a 1000 ml. cooled. funnel add 64 ml. If reaction starts. 1M hydrochloric acid and satd. using the remaing 10 inch piece gently poke at the magnesium turnings to expose fresh metal.34g. 20 mmol) in 20ml of toluene at -78°C and the mixture was under stirring allowed to slowly warm up to room temperature and refluxed for 12h. Aldrich). bp. Phenyl-2-Propanone by arylation of Potassium Acetylacetonate21 To a stirred solution of bromobenzene (31. isopropenyl acetate (9g. 167 mmol) and potassium acetylacetonate hemihydrate (125g.Phenyl-2-propanone was conveniently prepared from the enol ether by mixing with one equivalent of water with 0. This polymer is degraded to the monomer on distillation. Removal of the solvent gave 2.5% HCl and enough methanol to effect solution. sodium bicarb untill fizzing stops. stirred with 2M sodium hydroxide (250 ml) for 1 hr and extracted with toluene (2x500 ml). The mixture was stirred and heated at 100°C for 5 hr.

0. by Poodle: In a dream.) The solution was exposed for a vacuum to remove any remaining ether in the solution. to this was added 27g Mg turnings in portions.55 mol) in diethyl ether (100ml). there was added a solution of acetic anhydride (40g. This method could be of interest for producing P2P from acetonitrile. no chances was taken and 15 ml distilled water was added. followed by 50 ml brine. bp 214-215°C/760mmHg (100-101°C/13mmHg). The imine salt can also be reduced directly to amphetamine by sodium borohydride in methanol in high yield. To theresidue was added 100 ml. and so was decomposed to toluene. corresponding to a intermediate complex. of anhydrous benzene and the distillation was continued until about 50 ml. 52%). but after all was added. The reaction temperature rose to 30°C. as theoretically expected by a substance having a melting point at -16. the rxn mixture was cooled in an ice-salt bath.9g. washed.Submersion of the flask in cold H2O was used as necessary during addition to prevent excessive boiling of the Et2O. and 30. stirred thoroughly. The ketone was frozen at -20. there was excess unclogged Mg which would not react. stirring under reflux was continued for an additional hour. and no further reaction occurred. 0.] After all effervescence had stopped.4 grams (0. using constant swirling of the reaction mixture. After completion of addition. A thick white precipitate built up and clogged up some Mg. then acidified. the cooling bath removed and the reaction quenched by the careful addition of saturated aqueous ammonium chloride. the flask was cooled in an ice bath. After all Mg was added. it was still very orange even after adding NaCl and extracting with Et2O (which was a lighter shade of orange than the aq. Upon using the vaccum. The oily layer was separated and gave 21 ml of possible P2P. which was then extracted w/Et2O [NOTE: I think a lot of product was left behind in this aqueous layer. filtered. The benzylmagnesium chloride solution was added the acetonitrile over a periode of 10 minutes.2 mol) and magnesium shavings (4. After the addition after one hour was finished. prepared from benzyl chloride (25. not soluble in ether or acetonitrile. the mixture was refluxed gently. The organic phase was dried over MgSO4. The flask was again cooled in an ice bath and the reaction mixture decomposed by the addition of a solution of 25 grams of ammonium chloride in 200 ml of cold water.25 mole) of magnesium was stirred under reflux while 35. . the organic layer was separated. The intermediate phenyl-2-propanone imine magnesium salt can also be prepared from methylmagnesium iodide and benzyl cyanide. To this was added an etheral solution of benzylmagnesium chloride. responding to that temperature by forming a solid. Phenyl-2-Propanone by Grignard Addition to Acetic Anhydride26 In a 500-mL three-necked flask. Ether was removed by distillation on a steam bath. and washed twice with water-free ether to remove any unwanted remains of acetonitrile or benzyl chloride. a thermometer and an addition funnel (modified so that the added liquid was cooled externally by dry ice/acetone). and refluxed on a steam cone for 1 hour. so try to avoid it!].2 mol benzylmagesiumchloride grignard reagent were prepared by standard methods in diethylether (Total reaction volume: 200ml). [NOTE: This seemed to cause the Et2O layer to take on a reddish tint. as it greatly simplifies the procedure by eliminating any need for extensive extraction of the ketone. Simplification of the above procedure. Vacuum distillation of this oil afforded pure phenyl-2-propanone (bp 91-96°C at 11 mmHg). There was thus obtained 15. This complex was isolated by filtration through a buchner. situated in a dry ice/acetone slush in a Dewar flask. The reaction mixture was warmed to room temperature and refluxed with stirring on a steam cone for 1 hour. Both are hydrolyzed to phenyl-2-propanone with dilute hydrochloric acid. 2.2 mole) of phenylacetyl chloride in 75 ml of anhydrous benzene was added with stirring over a period of approximately 10 minutes. Reaction initiated by heating the mixture to 60°C for a short periode of time.5 grams (58%) of 1-phenyl-2-propanone. The benzene was removed by flash distillation and the ketone distilled under reduced pressure.to 10-minute period. more of distillate was collected. bp 74-76°C/3 mmHg). the reaction mixture was allowed to stir at dry ice temperature for 2-3 hours. and dried over anhydrous sodium sulfate. of anhydrous ether and 6. The organic phase was separated. About 2 moles of acetonitrile (100ml) was mixed with 100 ml of anhydrous diethylether and cooled in ice/water. and the flask was equipped with a magnetic stirrer. but as it began to turn yellow. of 62g acetonitrile in 100mL Et2O was added slowly while stirring w/a thermometer. the ether evaporated on a water bath and the residue fractionately distilled to yield phenyl-2-propanone (14g. layer!)]. A soln. then left to cool to room temp. an iodine crystal being added after the first portion to initiate Grignard rxn. 0. The combined Et2O layers were washed with H2O. A white percipitate was formed.9 grams (0. ether was removed and the solution separated into two layers with an orange oil on top and a water layer containing salts and undissolved salts. giving heat and causing remaining ether to boil. warmed to room temperature. I think the purity of final product would be higher if reaction mixture was first poured onto ice. The aqueous layer was separated. about 75-80% of the theoretical 26 ml. the organic phase washed with 10% sodium carbonate solution until the washes were no longer acidic to universal pH paper. the solution turned yellow/orange with oily orange bubbles. 500mL 10% HCl was added slowly under stirring.Phenyl-2-Propanone from Phenylacetyl Chloride and Dimethyl Cadmium32 A mixture of 40 ml. then another 10 ml (The complex reacted immediatly with the water.24 127g benzyl chloride was dissolved in 250mL Et2O.5 grams (0. Et2O and a small amount of toluene were evaporated to give 42g crude phenyl-2-propanone as a clear orange oil. The reaction mixture was cooled with an ice bath and 22.134 mole) of powdered anhydrous cadmium chloride was added over a 5.2 mol). Again 100 ml of anhydrous benzene was added.1 grams (0. [NOTE: This clogged-up material didn't react fully w/the MeCN. NaCl was added to the aqueous layer.25 mole) of methyl iodide in 140 ml. Phenyl-2-Propanone by Grignard addition to Nitriles19.5g. of anhydrous ether was added over a 3-hour period. The white complex was briefly dried. dried over MgSO4.

Chem. 733 (1989) Okabe. Shudo. 60. 82. Chemicke Listy 84(9). Syn. Practical Organic Chemistry. 21. p 391-392 Magidson and Garkusha. Khimii. if the ratio was less a considerable amount of acid was found in the product. 269 (1884) J. 612-613. T. 155-158 (1980) J.694. Lett. US Pat 3. Lett. Soc. Chem.Phenyl-2-Propanone from Benzylchloride (via dibenzyl cadmium)20. 2.. Shudo.16 mol) was added with vigorous stirring over 10-15 min. Ballini. and was allowed to stand without drying overight.. Pihkal #109 Okabe. 225. 62. Coll. Amer. Tet.2 mol benzyl chloride in 100ml anhydrous ether and 0. Synth. 1622 (1940) German Patents 3. K. 242 (1984) A. It was necessary to use a 2:1 molar ratio of the cadmium reagent to acid chloride. Frye. Anhydrous cadmium chloride (0. Stirring was continued with cooling for 2h. Jap.698 and 3. Abs. Soc. K. 5th Ed. 471). Tet. 60. 1050 (1927) US Patent 4. Chem. so keep it on ice during handling.232 Danilov and Danilova.2 mol magnesium turnings (Org. Syn.30. The solution of the grignard reagent was diluted with ether so that the concentration was no greater than 0. Vol 1. 68. The thermal stability of dibenzyl cadmium is low. Soc. McKillop.. 29(24). R. 5275-5280 (1970). The mixture was stirred in an ice-bath for 8h. Synthesis 723-726 (1994) J. Lett. A solution of 0. Vol.31 2 PhCH2MgCl + CdCl2 → (PhCH2)2Cd + 2 MgCl2 (PhCH2)2Cd + 2 CH3COCl → 2 PhCH2COCH3 + CdO Benzylmagnesium chloride was prepared from a solution of 0. 3777 (1985) Tet. Ber. 11(4) 339 (1941). Zh. Am.2 mol per 300ml and then cooled in an ice-bath.. Coulsen. Coll. 57.452. 5868 (1941) Chem. K. Oxidative Rearrangement of Olefins with Thallium(III)nitrate. 49. Tet. Vol. T.200.. Ohwada. J. Ohta.107 Alexander Shulgin. Lett.047 . Coll. 26. (bp 91-96°C at 11 mmHg). T. p 487-489 Org. Tetrahedron 46. H. I. References Org. 54. p. 993-4 (1990) US Pat 4. 3323-3326 (1964) Ann. Lett.629.1 mol acetyl chloride in 3 volumes anhydrous ether was added to the cold benzyl cadmium reagent over 5 min. 7539-7555 (1990) D. Chem. Org. Lett. Using benzyl cadmium chloride or dibenzyl cadmium gave little difference in yield. Ohta. Chem. A. T. 2112 (1935) Juraj Kizlink. Ohwada. The ether layer was separated and the aqueous phase extracted twice with ether. and hydrolyzed with 20% H2SO4.026.. The clear dark solution was filtered under nitrogen through a glass wool plug. The ether solution was then extracted with 4x25ml 10% sodium bicarbonate. Chem. Chem. Vogel. 2977-2978 (1988) R. Obsh. 45. and the residue vacuum distilled to give phenyl-2-propanone in 50-70% yield (calculated on the acid chloride). and all the pooled ether extracts were washed with water and dried over sodium sulfate. 1975 (1960) Chem. Chem. Org. Ber. 1603-1607 (1984) Tet. 597-600 (1982) Bull. A new Synthesis of Methyl Ketones. Oxidation of Olefinic Compounds with Solutions of Thallium(III) Salts. 2. The ether was distilled off. K. and the combined aqueous extracts were extracted twice with ether.541 [ Reference Lost ] A. The combined ether solutions were washed with water and 10% sodium bicarbonate. p.

Gilman. Oki. T. Analytical and many others. prenylamine. 37. methyl benzyl ketone. Alkyl Benzyl Ketones and Hydantoin Derivatives. T. We are leading Manufacturers and exporters of phenylacetone. and flavoring agents. Bulk Ordering & Pricing: Need larger quantities for your development. Engineering Data 15(1). Technical Service: Our team of scientists has experience in all areas of research including Life Science. 67. Chem. Trav. 1373-1381 (1985) Tet. Nelson. Due to the illicit uses in clandestine chemistry. Shiokawa. 741 (1939) H. we have adopted high level of operational quality standards that are strict on both the domestic as well as international market grounds. Org. prenylamine. We accept the complete responsibility for the process and quality aspects of each and every product we offer. It is clear oil with a refractive index of 1. . J.H. Often it's referred to as P2P (C9H10O) is an organic compound. rubber chemicals. February 1980. This commitment to quality and the obligation to our customers have been the foundation of our business since its inception. Rec. 200-201 (1970) I. 50. Phenylacetone shipment is available only to the importer who has import licence issued by Government. Electroreductive Acylation of Benzyl Chlorides with Acid Anhydrides. Chem. . alkaloids. Amer. 1-phenyl-(103-79-7) Benzyl methyl ketone(103-79-7) C9H10O 1-PHENYLACETONE1-PHENYL-2PROPANONEBENZYL METHYL KETONEPHENYLACETONEPHENYL-2-PROPANONE1phenyl-2-propanon1-phenyl-propan-2-one2-Propanone. benzyl methyl ketone. Chromatography. phenyl isopropyl amine. pargyline and estramustine. Scand. Often it's referred to as P2P) is an organic compound. fungicides. amphetamine. Lett. pargyline and estramustine.. suppliers & exporters of phenylacetone. Chim. 6.J.639.4methylenedioxymethamphetamine). Am. Chem.4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. Material Science. amphetamine. We are one of the leading manufacturers of fine chemicals. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. 782-790 (1952) J. Phenyl acetone family compounds are widely used as a parent compound to make drugs. Henze. 154 (1945) Acta Chem. 2451-2452 (1983) J. Phenylacetone shipment is available only to the importer who has import licence issued by Government.5168. manufacturing or research applications? Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine. Sund and H. it was declared a schedule II controlled substance in the United States 11. Soc. Chem. Soc. biocides. 518-530 (1936) E.4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. Org. Phenylacetone is called MDP2P (3. 24. phenyl isopropyl amine. Chemical Synthesis.R. benzyl methyl ketone or methyl benzyl ketone (Phenyl-2-propanone / Benzyl methyl ketone). F. Nishiguchi. J. commonly known as ecstasy. 55. Chem. Chemistry Letters 2005-2008 (1991) Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine. phenylacetone is also called phenyl-2-propanone. commonly known as ecstasy. 61. Hirashima and J.780 J. With prime focus on quality.4methylenedioxymethamphetamine). dyes. phenylacetone is also called phenyl-2-propanone. 3369-3370 (1972) US Pat 5. Phenylacetone is called MDP2P (3.

pargyline and estramustine. CAUTION : PHENYL ACETONE MAY BE A CONTROLLED COMMODITY IN YOUR COUNTRY Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine.3-indandione Warfarin Note: Reproduction of any materials from the site is strictly forbidden without permission. prenylamine. commonly known as ecstasy.4methylenedioxymethamphetamine).4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. Other use as an intermediate in the manufacture of Amphetamine Prenylamine Pargyline Estramustine Chlorophacinone & Diphacinone (rodenticides) . amphetamine. phenyl isopropyl amine. Active ingredients as anticoagulant include: Brodifacoum Chlorophacinone Coumachlor Difenacoum Diphacinane 2-Pivaloyl-1.3-indandione 2-Isovaleryl-1. Phenylacetone shipment is available only to the importer who has import licence issued by Government. Phenyl acetone is used as an intermediate to produce pesticides and anticoagulants.Phenyl acetone is structurally related to coumarine or cinnamic acid for the application of rodenticide anticoagulant and to phenethylamine which is a main structure in the activity of the sympathetic nervous system. Phenylacetone is called MDP2P (3.

10. Ltd in India. (India)All Rights Reserved. . G.1019. The above information is believed to be correct but does not purport to be all-inclusive and shall be used only as a guide. Contact information for MulBerry Chemicals Pvt. Chemicals Manufacturers In India ®™* Trademark of The MulBerry Chemicals Pvt. 487-489 K. . . 417-421 °F *** Reproduction of any materials from the site is strictly forbidden without permission. 258 K.Valsad.Sarigam. Road No. MulBerry Chemicals Pvt. Dist. Ltd . 5 °F 214-216 °C.006 g/mL -15 °C.Phenylacetone 1-phenylpropan-2-one Other names benzyl methyl ketone.D. Ltd ("Mulberry Chemicals") or an affiliated company of MBC. Plot No. Pin Code . methyl benzyl ketone.I. Shall not be held liable for any damage resulting from handling or from contact with the above product. phenyl-2propanone Identifiers CAS number 103-79-7 PubChem 7678 ChemSpider 21106366 UNII O7IZH10V9Y KEGG C15512 ChEBI CHEBI:52052 Molecular formula Molar mass Densit y Melting point Boiling point Properties C 9H10O 134. . State of Gujrat.18 g mol. Vill.C.1 1.396142 © 2009-2011. .