HRID36591

反应详情

EQUATION

反应方程式

HRID 36591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of glyoxylic acid monohydrate (23 g, 250 mmol), propargyl alcohol (16.8 g, 300 mmol ), copper (II) chloride (3.2 g, 25 mmol) and ammonium acetate (49 g, 600 mmol) in ethanol (100 ml) is heated under reflux for 6 h. Then the reaction mixture is concentrated in vacuo, diluted with water (50 ml), acidified to pH 5 with 1N HCl and washed twice with ether (100 ml). Then the aqueous solution is poured on an ion exchange resin column (DOWEX 50, H+) The column is eluted with 1M ammonium hydroxide to give the title compound 2-amino-5-hydroxy-3-pentynoic acid.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 6 h
  3. concentrationThen the reaction mixture is concentrated in vacuo
  4. additiondiluted with water (50 ml)
  5. washwashed twice with ether (100 ml)
  6. additionThen the aqueous solution is poured on an ion exchange resin column (DOWEX 50, H+) The column
  7. washis eluted with 1M ammonium hydroxide