反应详情

A solution of 2-cyano-5-pyridylmethyl chloride (4.6 g) in acetonitrile (20 ml) was added dropwise at 5° to 10° C. to a solution of ethylenediamine (9 g) in acetonitrile (50 ml). 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 mixture. Dichloromethane was added to the residue, and a portion soluble in dichloromethane was recovered. Dichloromethane was distilled off under reduced pressure, and 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 mixture
3. additionDichloromethane was added to the residue
4. customa portion soluble in dichloromethane was recovered
5. distillationDichloromethane was distilled off under reduced pressure, and volatile materials
6. customwere removed at 50° C.