HRID19368

反应详情

EQUATION

反应方程式

HRID 19368 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 solution of 3-(2-chloro-phenoxy)-4-((S)-3-methoxy-1-methoxycarbonyl-propylamino)-but-2-enoic acid ethyl ester (112 mg, 0.29 mmol) in acetonitrile (2 mL) was placed in a sealed microwave reaction tube and heated in a microwave reactor at 130° C. for 2 h, 150° C. for 2 h, and 160° C. for 3 h. The mixture was then concentrated in vacuo and purified by AnaLogix IntelliFlash flash chromatography (8 g column, 20% ethyl acetate/hexanes to 70% ethyl acetate/hexanes) which afforded (S)-2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methoxy-butyric acid methyl ester (71 mg, 39% over two steps) as a clear colorless oil.

WORKUP

后处理

  1. concentrationThe mixture was then concentrated in vacuo
  2. custompurified by AnaLogix IntelliFlash flash chromatography (8 g column, 20% ethyl acetate/hexanes to 70% ethyl acetate/hexanes) which