HRID1620560

反应详情

EQUATION

反应方程式

HRID 1620560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of the obtained 7-oxoazepane-4-carboxylate (2.02 g) in THF (29 mL) was added dropwise to a suspension of lithium aluminum hydride (2.07 g) in THF (80 mL) under ice-cooling. The reaction mixture was stirred at room temperature for 3 hr and at 60° C. overnight. The reaction mixture was ice-cooled, diluted with THF (200 mL), and water (2.02 mL) was slowly added dropwise. Furthermore, 15% aqueous sodium hydroxide solution (2.02 mL) was added dropwise, then water (4.04 mL) was added, and the mixture was stirred at room temperature for 3 hr. The solid was separated by filtration, and the filtrate was concentrated under reduced pressure to give the title compound (1.41 g).

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooled
  3. additionwas slowly added dropwise
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. customThe solid was separated by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure