反应详情

m-Cyanobenzylamine (13.2 g), water (18 g), and 1,2-dichloroethane (22 g) were mixed, and the mixture was stirred with cooling with ice. Acetic acid (18 g) was added to the mixture. Subsequently, a 20 wt % aqueous solution (51.8 g) of sodium nitrite was added dropwise to the mixture over a one hour period. The mixture was stirred at the same temperature for four hours. The reaction mixture was subjected to extraction with 1,2-dichloroethane, and the organic solvent was concentrated. Water was added to the concentrated solution, and the residual organic solvent was removed through distillation, to thereby obtain 13.7 g of m-cyanobenzyl acetate (yield 78%). The purity of the product was 97%.

1. temperaturewith cooling with ice
2. stirringThe mixture was stirred at the same temperature for four hours
3. extractionThe reaction mixture was subjected to extraction with 1,2-dichloroethane
4. concentrationthe organic solvent was concentrated
5. additionWater was added to the concentrated solution
6. customthe residual organic solvent was removed through distillation