HRID1731051

反应详情

EQUATION

反应方程式

HRID 1731051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.8 g. (6 mmol.) of N-(β,β,β-trichloroethoxycarbonyl)-2-acetoxyglycine n-butyl ester and 1.2 g. (10 mmol.) of 2,6-dimethylphenol in 20 ml. of methylene chloride containing 3 drops of boron trifluoride etherate was stirred at 25° for 3 hours. The reaction mixture was concentrated in vacuo, 5 ml. of 2:1 hexanemethylene chloride was added and the resulting solution was chromatographed on silica gel. Elution with 2:1 hexanemethylene chloride then with methylene chloride containing increasing amounts of ethyl acetate gave the title compound.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo, 5 ml
  2. additionof 2:1 hexanemethylene chloride was added
  3. customthe resulting solution was chromatographed on silica gel
  4. washElution with 2:1 hexanemethylene chloride
  5. temperaturewith methylene chloride containing increasing amounts of ethyl acetate