HRID467132

反应详情

EQUATION

反应方程式

HRID 467132 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-50 °C

PROCEDURE

实验过程

A cooled and freshly distilled solution of 270 mg of pyruvic acid in 5 ml of chloroform is rapidly stirred into a solution of 700 mg of Tic-OBut and 630 mg of dicyclohexylcarbodiimide in 15 ml of anhydrous chloroform, the latter solution having been cooled to -50° C. The mixture is left for 16 hours in a deep-freezing cabinet (-20° C.), and the precipitated dicyclohexylurea is filtered off. The solution is washed with KHSO4 solution and then with KHCO3 solution, dried over Na2SO4, and concentrated in vacuo. The compound (oil) contains a little dicyclohexylurea, and was analyzed by chromatography over silica gel in the system CHCl3 /CH3OH 15:1.

WORKUP

后处理

  1. temperatureA cooled
  2. filtrationthe precipitated dicyclohexylurea is filtered off
  3. washThe solution is washed with KHSO4 solution
  4. dry with materialwith KHCO3 solution, dried over Na2SO4
  5. concentrationconcentrated in vacuo