Organic Syntheses by Unknown
page 68 of 106 (64%)
page 68 of 106 (64%)
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[4] D. R. P. 25,469; Frdl. 1, 335 (1883).
[5] Ber. 33, 806 (1900). [6] J Chem. Soc. 32, 47 (1877); Ann. 189, 146 (1877). XVII PHENYLACETIC ACID C6H5CH2CN + 2H2O + H2SO4--> C6H5CH2CO2H + NH4HSO4 Prepared by ROGER ADAMS and A. F. THAL. Checked by O. KAMM and A. O. MATTHEWS. 1. Procedure IN a 5-l. round-bottom flask, fitted with a mechanical stirrer and reflux condenser, are mixed 1150 cc. of water, 840 cc. of commercial sulfuric acid and 700 g. of benzyl cyanide (preparation III, p. 9). The mixture is heated under a reflux condenser and stirred for three hours, cooled slightly and then poured into 2 l. of cold water. The mixture should be stirred so that a solid cake is not formed; the phenylacetic acid is then filtered off. This crude material should be melted under water and washed by decantation several times with hot water. These washings, on cooling, deposit a small amount of phenylacetic acid which is filtered off and added to the main portion of material. |
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