HRID1706591

反应详情

EQUATION

反应方程式

HRID 1706591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 12.4 g (0.10 moles) of 3-hydroxy-3-methylglutaronitrile in 107 ml of 1.3 M sodium hydroxide is stirred at room temperature while 17.4 ml (0.20 moles) of 30% hydrogen peroxide is slowly added. After the addition of peroxide, the mixture is heated to boiling and boiling is maintained for 2 hours. Thereafter the mixture is cooled, diluted to 1 liter with water and passed through a 200 ml column of Dowex 2 resin in the formate form. The column is then washed with 1 liter of water. Thereafter the product is eluted with 1 liter of 0.1 N formic acid and the eluate evaporated to dryness to afford 3-hydroxy-3-methylglutaric acid monoamide.

WORKUP

后处理

  1. additionis slowly added
  2. temperaturethe mixture is heated
  3. temperatureboiling is maintained for 2 hours
  4. temperatureThereafter the mixture is cooled
  5. washThe column is then washed with 1 liter of water
  6. washThereafter the product is eluted with 1 liter of 0.1 N formic acid
  7. customthe eluate evaporated to dryness