反应详情

A solution of 2-cyano-5-pyridylmethyl chloride (4.6 g) in acetonitrile (20 ml) was added dropwise to a solution of ethylenediamine (9 g) in acetonitrile (50 ml) at 5 to 10° C. After the addition, the mixture was stirred at room temperature for 3 hours. Acetonitrile and the excess of ethylenediamine were distilled off under reduced pressure from the reaction mixture. Dichloromethane was added to the residue, and a portion of it soluble in dichloromethane was separated. Dichloromethane was distilled off under reduced pressure. Volatile materials were removed at 50° C. and 1 mmHg to give N-(2-cyano-5-pyridylmethyl)ethylenediamine (4.5 g) as a colorless oil.

1. additionAfter the addition
2. distillationAcetonitrile and the excess of ethylenediamine were distilled off under reduced pressure from the reaction mixture
3. additionDichloromethane was added to the residue
4. customa portion of it soluble in dichloromethane was separated
5. distillationDichloromethane was distilled off under reduced pressure
6. customVolatile materials were removed at 50° C.