反应详情

温度

20 °C

N-(3-Methylbutyl)-10-[(2RS)-1-(N-ethyl-N-methyl-amino)-2-propyl]-2-phenothiazinecarbothioamide (0.3 g) is dissolved in a solution of fumaric acid (81 mg) in absolute ethanol (5 cc) and the mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residual orange product of meringue-like consistency is dissolved in acetic acid (5 cc) and mercuric acetate (0.23 g) is added. The orange suspension obtained is stirred for 16 hours at a temperature in the region of 20° C. The reaction mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 60° C. The residue is taken up with distilled water (10 cc) and filtered and the filtrate is alkalinized with caustic soda (d=1.33) to pH 13 and extracted with ethyl acetate (2×10 cc). The combined organic phases are washed with saturated aqueous sodium chloride solution (10 cc), dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residual yellow oil (0.15 g) is dissolved in ethyl acetate (2 cc), and isopropyl ether (20 cc) is added. The solution obtained is cooled to a temperature in the region of 5° C. and a solution (5.1 cc) of 0.065N hydrochloric acid in isopropyl ether is added dropwise and with stirring. The precipitate formed is drained, washed with isopropyl ether (3×5 cc) and dried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C. N-(3-Methylbutyl)-10-[(2RS)-1-(N-ethyl-N-methylamino)-2-propyl]-2-phenothiazinecarboxamide hydrochloride (0.13 g) is thereby obtained in the form of an off-white solid, m.p. 110-120° C. (melts forming a paste).

1. concentrationthe mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
2. dissolutionThe residual orange product of meringue-like consistency is dissolved in acetic acid (5 cc)
3. additionmercuric acetate (0.23 g) is added
4. customThe orange suspension obtained
5. concentrationThe reaction mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 60° C
6. filtrationfiltered
7. extractionextracted with ethyl acetate (2×10 cc)
8. washThe combined organic phases are washed with saturated aqueous sodium chloride solution (10 cc)
9. dry with materialdried over magnesium sulphate
10. filtrationfiltered
11. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
12. dissolutionThe residual yellow oil (0.15 g) is dissolved in ethyl acetate (2 cc)
13. additionisopropyl ether (20 cc) is added
14. customThe solution obtained
15. temperatureis cooled to a temperature in the region of 5° C.
16. stirringwith stirring
17. customThe precipitate formed
18. washwashed with isopropyl ether (3×5 cc)
19. customdried under reduced pressure (5 mm Hg; 0.7 kPa) at 40° C