反应详情

温度

25 °C

Thionyl chloride (5.2 cc) is added to a suspension, cooled to 5° C., of 10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxylic acid hydrochloride (3.9 g) in methylene chloride (120 cc). The suspension is stirred for 3 hours at 25° C. and then concentrated to dryness at 30° C. under reduced pressure (30 mm Hg; 4 kPa) to give a yellow residue which is taken up in methylene chloride (50 cc) at 5° C. Cyclopentylamine (5 cc) is added and the mixture is stirred for 12 hours at 25° C., and saturated sodium bicarbonate solution (150 cc) is then added. The mixture is extracted with ethyl acetate (2×100 cc). The organic phase is washed successively with distilled water (100 cc) and with brine (100 cc), dried over magnesium sulphate, filtered and concentrated to dryness at 40° C. under reduced pressure (30 mm Hg; 4 kPa) to give a yellow oil which is dissolved in boiling acetonitrile (70 cc). Crystallization is primed by scratching. After cooling, the solid is separated by filtration, washed with acetonitrile (2×3 cc) and dried at 40° C. under reduced pressure (1 mm Hg; 0.13 kPa). N-Cyclopentyl-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide (2.1 g) is obtained in the form of cream-coloured crystals, m.p. 132° C.

1. concentrationconcentrated to dryness at 30° C. under reduced pressure (30 mm Hg; 4 kPa)
2. customto give a yellow residue which
3. stirringthe mixture is stirred for 12 hours at 25° C.
4. extractionThe mixture is extracted with ethyl acetate (2×100 cc)
5. washThe organic phase is washed successively with distilled water (100 cc) and with brine (100 cc)
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. concentrationconcentrated to dryness at 40° C. under reduced pressure (30 mm Hg; 4 kPa)
9. customto give a yellow oil which
10. dissolutionis dissolved
11. customCrystallization
12. temperatureAfter cooling
13. customthe solid is separated by filtration
14. washwashed with acetonitrile (2×3 cc)
15. customdried at 40° C. under reduced pressure (1 mm Hg; 0.13 kPa)