Freshly distilled phenylacetaldehyde ( Note 1 ) and.
The organic layer is separated and redistilled to give pure phenyl-2-propanone, bp 105C/10 mmHg or 216C at atmospherical pressure.
Ephedrine derivatives that can be used in this procedure include Ephedrine, Pseudoephedrine, Norephedrine and Norpseudoephedrine (Phenylpropanolamine).Reduction with Iron Powder 13 If phenyl-2-nitropropene is reduced by iron powder in an acidic medium (such as acetic acid or aqueous hydrochloric acid) the quirumed code promo nitroalkene is reduced to the code de reduction last minute 2018 oxime, which is then hydrolyzed by the acid into the desired phenyl-2-propanone.The benzylmagnesium chloride solution was added the acetonitrile over a periode of promo renault twingo 10 minutes, using constant swirling of the reaction mixture.The ylid resulting from treatment of the phosphonium salt with base was found to be very unstable at room tempature, the characteristic red color dissappearing within a few seconds.The ether layer was separated and the aqueous phase extracted twice with ether.The 2,4 dinitrophenylhydrazone derivative, recrystallized from methanol, had mp 152.5-153.5C.Welcome to the world of P2P.Yield 50-55 ml, 85 of P2P.Triflic Acid Method 14 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 -40C in a dry ice-acetone bath.
The reaction mixture was poured into 2000ml water, and was extracted with 3x100 ml CH2Cl2.Many other metal salts can be used instead of the zinc chloride, for details, see the translation of the original patents.The yield about 30ml (70).At 145C the stream of steam is increased, and during.5-3 hours the phenylacetone is steam distilled from the reaction mixture.The benzene layer was separated and the aqueous layer extracted with four 25 ml portions of benzene.The ether solution was then dried over magnesium sulphate, filtered and the ether driven off, first at ordinary pressure and then at aspirator vacuum to give.65g (76) of phenylacetone, usually pure enough for most purposes.Electrosynthesis of P2P from Benzyl Chloride 4 Synthesis of phenyl-2-propanone from benzyl chloride (79 mmol) and acetic anhydride (686 mmol) by electrolysis of the reaction mixture.Phenyl-2-propanone by nitroalkylation of benzene Titanium Tetrachloride Method 7 To a stirred solution of 2-nitropropene (0.1 mol,.7g) in dry CH2Cl2 (300ml) was added benzene (0.5 mol, 39g) at room temperature.Phenyl-2-Propanone from Chloroacetone 9 41 grams (0.31 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, a reflux water condenser and a small addition funnel.The ether was then dried over anhydrous Na2SO4 (or MgSO4 the solvent evaporated and the residue fractionately distilled to recover unreacted benzene, and to give phenyl-2-propanone in 40 yield (1.34g) based on the reacted manganese(III)acetate, which is the limiting reagent in this reaction.
Potassium Acetate/Copper Sulfate 3c To a mixture of 136 g (1.0 mol) phenylacetic acid, 70 g sodium or potassium acetate, and 16 g (0.1 mol) anhydrous cupric sulphate is introduced 2000 ml anhydrous acetic anhydride in 4000 ml flask.
Ether was removed by distillation on a steam bath.
All of the precipitate was also be gone at this point.