HRID1075219

反应详情

EQUATION

反应方程式

HRID 1075219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 230 mg (0.40 mmole) of (3S, 4R)-3-[(R)-1-t-butyldimethylsilyloxyethyl]-4-[1-methyl-2-p-nitrobenzyloxycarbonylaminoethylthio(thiocarbonyl)]thioazetidin-2-one, 182 mg (0.80 mmole) of p-nitrobenzyl glyoxylate hydrate and 5 ml of benzene was heated under reflux for 10 hours. After completion of the reaction the solvent was distilled off and the resulting residue was subjected to column chromatography through 10 g of silica gel eluted with a 7-10% v/v solution of ethyl acetate in benzene to afford 234 mg (yield 75%) of the desired product as a yellow oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 10 hours
  3. customAfter completion of the reaction the solvent
  4. distillationwas distilled off
  5. washeluted with a 7-10% v/v solution of ethyl acetate in benzene