HRID413748

反应详情

EQUATION

反应方程式

HRID 413748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 3-cyanamidobenzotrifluoride (1.20 g, 6.45 mmol) and 4-chlorobenzylamine hydrochloride (1.26 g, 7.09 mmol) was stirred at 150° C. for 40 h. Dichloromethane (100 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 1.05 g, 50%. M.p. 103-105° C.

WORKUP

后处理

  1. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml)
  2. customThe organic phase was purified by chromatography
  3. additiona mixture of methanol (10%) and dichloromethane as eluent
  4. customThe product was isolated as the free base