HRID974401

反应详情

EQUATION

反应方程式

HRID 974401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

71.6 g (0.50 mol) of 2,4-difluorobenzylamine, 100.2 g (1.0 mol) of caproaldehyde, 1.0 g of acetic acid, 10 g of Raney nickel in ethanol and 500 ml of tetrahydrofuran are introduced into a 1 l autoclave. This mixture is heated to 100° C. and hydrogenated with stirring and under a pressure of 100 bar. After 13 hours, the take-up of hydrogen is 142% of theory. The black suspension is filtered, and the filtrate is evaporated on a rotary evaporator and subsequently distilled at 77° C. and 2 mbar. 33.1 g of a colourless liquid are obtained.

WORKUP

后处理

  1. filtrationThe black suspension is filtered
  2. customthe filtrate is evaporated on a rotary evaporator
  3. distillationsubsequently distilled at 77° C.