HRID1894850
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of 5 g (25 mmol) of 1-phenylaminocyclohexanecarbonitrile in 70 ml of ethyl ether is added drop by drop to 1.13 g (29.8 mmol) of lithium aluminum hydride in 30 ml of ethyl ether at 0° C. The mixture is stirred for 2 hours at 0° C. The reaction is stopped by the addition of 1.1 ml of water, 1.1 ml of 15% sodium hydroxide and then 3.5 ml of water. The medium is then filtered on Celite and the filtrate is evaporated. The residue is purified on silica gel (dichloromethane then dichloromethane/methanol 80/20, v/v). 2 g of (1-aminomethylcyclohexyl)phenylamine are obtained in the form of a brown oil. Yield=39%.
WORKUP
后处理
- filtrationThe medium is then filtered on Celite
- customthe filtrate is evaporated
- customThe residue is purified on silica gel (dichloromethane