HRID1940207

反应详情

EQUATION

反应方程式

HRID 1940207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To tetrahydrofuran (20 ml) were added (3R,5S)-7-Chloro-5-(2-chlorophenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid (2 g) and aluminum lithium hydride (0.4 g). The mixture was heated for 6 hours under reflux, to which was added water. Insolubles were then filtered off. The filtrate was concentrated, which was purified by means of a silica gel column chromatography (hexane:acetic acid ethyl ester=2:1 v/v as an eluent) to give 1.65 g of non-crystalline solid matter.

WORKUP

后处理

  1. temperatureThe mixture was heated for 6 hours
  2. temperatureunder reflux, to which
  3. filtrationInsolubles were then filtered off
  4. concentrationThe filtrate was concentrated
  5. customwhich was purified by means of a silica gel column chromatography (hexane