In a 1-l. three-necked round-bottomed flask fitted with a Hershberg stirrer and a constant water separator (Note 1) surmounted by a reflux condenser are placed 120 g. (1 mole) of acetophenone, 113 g. (1 mole) of ethyl cyanoacetate (Note 2), 15.4 g. (0.2 mole) of ammonium acetate, 48.0 g. (0.8 mole) of glacial acetic acid, and 200 ml. of benzene. The reaction mixture is stirred and heated under reflux for 9 hours during which time 28–33 ml. of lower layer is collected in the water separator (Note 3). To the cooled reaction mixture is added 100 ml. of benzene, and the whole is extracted with three 100-ml. portions of water. The combined aqueous layers are extracted with 30 ml. of benzene, which is then added to the organic layer from the previous extraction. Anhydrous magnesium sulfate (15 g.) is added, and, after swirling occasionally for 10 minutes, the mixture is filtered by suction and the magnesium sulfate washed with two 25-ml. portions of benzene. The benzene is removed by distillation at reduced pressure and the residual oil distilled rapidly through a 15-cm. column. The yield of ester is 113–125 g. (52–58%), b.p. 135–160° (0.35 mm.) (Note 4).