HRID704238

反应详情

EQUATION

反应方程式

HRID 704238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10-[(2RS)-1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride (3.72 g) is added to a solution of potassium hydroxide (1.7 g) in glycol (20 cc), and the mixture is stirred for 5 hours under reflux. After cooling, the yellow solution obtained is traeted with a 3N ethereal solution (10 cc) of hydrochloric acid, and diluted with acetone (100 cc) and ethyl ether (100 cc) and then filtered. The yellow filtrate, after priming, gives rise to the crystallization of a product, which is drained, washed with ethyl ether (2×10 cc) and dried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C. 10-[(2RS)-1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride (3.5 g) is thereby obtained in the form of pale yellow crystals, m.p. 215°-217° C.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. customthe yellow solution obtained
  4. filtrationfiltered
  5. customThe yellow filtrate, after priming, gives rise
  6. customto the crystallization of a product, which
  7. washwashed with ethyl ether (2×10 cc)
  8. customdried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C