HRID845169

反应详情

EQUATION

反应方程式

HRID 845169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

By using a method similar to that described in Example 35, but starting from 3-dimethylaminoacrylophenone (6.1 g), phosphorus oxychloride (3 cc), 2-chlorothiophenol (5 g) and sodium cyanoborohydride (1.3 g), and after evaporating the organic phase to dryness under reduced pressure (2.7 kPa) at 40° C., a yellow oil is obtained which is dissolved in isopropanol (20 cc). A 5.6N solution (7.8 cc) of hydrochloric acid gas in ethyl ether is added to this solution. The precipitate formed is separated off by filtration and then recrystallised from isopropanol (20 cc). In this way 3-(2-chlorophenylthio)-1-dimethylamino-3-phenyl-2-propene (Z) hydrochloride (2.5 g) is obtained in the form of a white solid melting at 162° C.

WORKUP

后处理

  1. customafter evaporating the organic phase to dryness under reduced pressure (2.7 kPa) at 40° C.
  2. customa yellow oil is obtained which
  3. customThe precipitate formed
  4. customis separated off by filtration
  5. customrecrystallised from isopropanol (20 cc)