HRID704228

反应详情

EQUATION

反应方程式

HRID 704228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Aluminium chloride (0.5 g) and sulphuryl chloride (39.7 cc) are added in the course of 4 hours to a solution, heated to 50° C., of 2-phenothiazinecarbonitrile (100 g) in 1,2-dichloroethane (3000 cc). The reaction mixture is brought to reflux for 2 hours, and then stirred for 48 hours at 25° C. The precipitate formed is filtered off, washed with 1,2-dichloroethane (2×200 cc) and then with ethyl ether (200 cc) and dried at 40° C. under reduced pressure (30 mm Hg; 4 kPa) to give 7-chloro-2-phenothiazinecarbonitrile (69.3 g) in the form of a yellow-green solid, m.p. 235° C.

WORKUP

后处理

  1. temperatureto reflux for 2 hours
  2. customThe precipitate formed
  3. filtrationis filtered off
  4. washwashed with 1,2-dichloroethane (2×200 cc)
  5. dry with materialwith ethyl ether (200 cc) and dried at 40° C. under reduced pressure (30 mm Hg; 4 kPa)