HRID1181440

反应详情

EQUATION

反应方程式

HRID 1181440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a suspension of 4-(morpholin-4-ylmethyl)benzonitrile (Description 122, 0.5 g, 2.5 mmol) in THF (7 mL) at 0° C. was added dropwise a solution of LiAlH4 (1.0 M in THF, 2.5 ml, 2.5 mmol). The reaction was stirred at 0° C. for 1 h. Additional LiAlH4 (1.0 M in THF, 1.0 ml, 1.0 mmol) was added and the reaction stirred for an additional 30 min. The reaction was quenched by the addition of water (0.13 mL) followed by 15% NaOH solution (0.13 ml) and stirred vigorously for 1 h. The reaction was filtered through celite, evaporated and azeotroped twice with toluene. The amine was used crude.

WORKUP

后处理

  1. stirringthe reaction stirred for an additional 30 min
  2. customThe reaction was quenched by the addition of water (0.13 mL)
  3. stirringstirred vigorously for 1 h
  4. filtrationThe reaction was filtered through celite
  5. customevaporated
  6. customazeotroped twice with toluene