反应详情

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 cooling, 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 seeding, crystallization is allowed to take place for 15 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 light yellow solid, m.p. 200° -210° C. (melts forming a paste).

1. temperatureunder reflux
2. temperatureAfter cooling
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. customcrystallization
7. customfor 15 hours
8. customin the region of 5° C
9. customThe solid obtained
10. washwashed with ethyl ether (10 cc)
11. customdried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C