HRID620406

反应详情

EQUATION

反应方程式

HRID 620406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of hydroxylamine hydrochloride (5.09 g, 72 mmol) in methanol (26 ml) was added to a solution of 88% potassium hydroxide (6.99 g, 109 mmol) in methanol (15.3 ml), keeping the temperature below 40° C. The mixture was cooled to 0° C., filtered, and methyl 3,4-dimethoxycinnamate (8.0 g, 36 mmol) was added to the filtrate. After two hours, concentrated HCl (5 ml) was added to the cold solution. The resulting precipitate was filtered, washed with water and ether, and dried in vacuo, to give 6.74 g (84% yield) of the named compound, mp 183°-185° C.

WORKUP

后处理

  1. customthe temperature below 40° C
  2. filtrationfiltered
  3. filtrationThe resulting precipitate was filtered
  4. washwashed with water and ether
  5. customdried in vacuo