HRID728736

反应详情

EQUATION

反应方程式

HRID 728736 的结构方程式

PROCEDURE

实验过程

10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarbonitrile hydrochloride, L series (5 g) is added to a solution of potassium hydroxide (1.75 g) in glycol (30 cc), and the mixture is stirred for 4 hours under reflux. After being cooled, the yellow solution obtained is diluted with acetone (75 cc) and a 3N solution (5 cc) of hydrochloric acid in ethyl ether, filtered and diluted again with acetone (75 cc) and a 3N solution (5 cc) of hydrochloric acid in ethyl ether. After priming, the mixture is left to crystallize for 16 hours at a temperature in the region of 5° C. The solid obtained is drained, washed with ethyl ether (10 cc) and dried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C. 10-[1-(1-Pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride, L series (2.9 g) is thereby obtained in the form of a pale yellow solid, m.p. 200-210° C. (melts forming a paste).

WORKUP

后处理

  1. temperatureunder reflux
  2. temperatureAfter being cooled
  3. customthe yellow solution obtained
  4. filtrationa 3N solution (5 cc) of hydrochloric acid in ethyl ether, filtered
  5. additiondiluted again with acetone (75 cc)
  6. waitthe mixture is left
  7. customto crystallize for 16 hours at a temperature in the region of 5° C
  8. customThe solid obtained
  9. washwashed with ethyl ether (10 cc)
  10. customdried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C