反应详情

温度

20 °C

Fumaric acid (2.7 g) is added to a solution of N-propyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide, L series (9.5 g) in ethanol (100 cc). The solution obtained is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The merigue-like yellow residue is taken up with acetic acid (200 cc). Mercuric acetate (7.3 g) is added to the solution obtained, and the mixture is stirred for 16 hours at a temperature in the region of 20° C. The black suspension obtained is diluted with distilled water (200 cc) and filtered. The yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residue is taken up with ethyl acetate (250 cc) and distilled water (50 cc) and then treated with sodium hydroxide (d 1.33) to pH 13. The aqueous phase is separated after settling has taken place and extracted with ethyl acetate (250 cc). The organic phases are combined, washed successively with distilled water (2×100 cc) and with saturated aqueous sodium chloride solution (100 cc) and dried over magnesium sulphate. After filtration, the yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. and a crude yellow oil (9.2 g) is thereby obtained. This residue is purified by chromatography on a column (height: 22 cm; diameter: 4 cm) of silica gel (0.2-0.063 mm), eluting with a mixture (95:5 by volume) of methylene chloride and methanol. The first 1,500 cc are discarded and the next 1,500 cc are concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give N-propyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide, L series (7.3 g) in the form of a yellow gum.

1. customThe solution obtained
2. concentrationis concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
3. additionMercuric acetate (7.3 g) is added to the solution
4. customobtained
5. customThe black suspension obtained
6. filtrationfiltered
7. concentrationThe yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C
8. distillationdistilled water (50 cc)
9. additiontreated with sodium hydroxide (d 1.33) to pH 13
10. customThe aqueous phase is separated after settling
11. extractionextracted with ethyl acetate (250 cc)
12. washwashed successively with distilled water (2×100 cc) and with saturated aqueous sodium chloride solution (100 cc)
13. dry with materialdried over magnesium sulphate
14. filtrationAfter filtration
15. concentrationthe yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
16. customa crude yellow oil (9.2 g) is thereby obtained
17. customThis residue is purified by chromatography on a column (height: 22 cm; diameter: 4 cm) of silica gel (0.2-0.063 mm)
18. washeluting with a mixture (95:5 by volume) of methylene chloride and methanol
19. concentrationthe next 1,500 cc are concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C.