HRID1155969

反应详情

EQUATION

反应方程式

HRID 1155969 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thionyl chloride (4.2 g) in diethyl ether (10 ml) was added dropwise with stirring at 0°-5° C. to a solution of 2-(5-cyano-2-hydroxyphenyl)-2-methyl-1-propanol (5 g) prepared as in Example 26, and pyridine (5.5 g) in diethyl ether (80 ml). The mixture was stirred for 3 hours at 0°-20° C. Water was then added and the mixture was filtered. The ether solution was then washed with dilute hydrochloric acid, then with aqueous sodium bicarbonate and water (twice), then dried over magnesium sulphate and run down. The residue was recrystallised from ethanol, giving the title product (2.0 g) as white crystals, mp 87°-88° C.

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. washThe ether solution was then washed with dilute hydrochloric acid
  3. dry with materialwith aqueous sodium bicarbonate and water (twice), then dried over magnesium sulphate
  4. customThe residue was recrystallised from ethanol