Modified Claisen flask with a 25 cm fractionating side arm. The ether is removed from the filtrates, and the residue distilled from a Sodium sulfate is collected on a filter, washed with ether, and discarded. The oil andĮther layers are washed successively with 100ml of water, the ether combined with the oil and dried over 20g of anhydrous sodium sulfate. The ketone forms a layer and, after cooling, is separated and the acid layer extracted with 600ml of ether. The solution is cooled to 0☌, 1750ml of water added rapidly, and the flask placed on a vigorously boiling water bath and heated for two hours, with After all is added the flask is warmed on the steam bath until solution is complete and then for five minutes longer.
Kept below 20☌ (If pure dry alpha-phenylacetoacetonitrile is used, half its weight of water should be added to the sulfuric acid or charring will Obtained according to the procedure above (corresponding to 188-206g or 1.2-1.3 moles of dry product) is added slowly, with shaking, the temp being The total first crop of moist alpha-phenylacetoacetonitrile Of dry colorless alpha-phenylacetoacetonitrile, mp 87-89☌.ģ50 ml of concentrated sulfuric acid is placed in a 3000ml flask and cooled to -10☌. The moist cake weighing about 300g corresponds to 188-206g (59-64%) Suction filtration and washed four times on the funnel with 250 ml portions of water. Precipitated by adding slowly, with vigorous shaking, 90 ml of glacial acetic acid, while the temperature is kept below 10☌. The sodium salt still wet with ether is dissolved in 1.3 liters of distilled water at room temperature, the solution cooled to 0☌, and the nitrile The combined filtrates are placed in the freezing mixture until they can be The filter cake is practically colorless andĬorresponds 250-275g of dry sodium salt, or 69-76% of the calculated mount. The sodium salt isĬollected on a 6 inch Buchner funnel and washed four times on the funnel with 250 ml portions of ether. Mixture is stirred with a wooden rod to break lumps, cooled in a freezing mixture to -10☌, and kept at this temperature for two hours. The mixture is thoroughly shaken, theĬondenser closed with a calcium chloride tube, 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 benzylĬyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P 2O 5 for 30min followed by distillation). (2.6 mol) clean sodium and 700 ml of absolute alcohol (dried over calcium oxide or sodium) in aĢ000 ml round-bottomed flask equipped with a reflux condenser.
Phenyl-2-propanone (also called P2P, BMK, Benzyl Methyl Ketone or Phenylacetone).
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