反应详情

温度

100 °C

A suspension of 10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide (2 g) and pentylamine (3 cc) in absolute ethanol (30 cc) is saturated with hydrogen sulphide and then heated for 2 hours at a temperature in the region of 100° C. After cooling, the mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The pasty residue is taken up with ethyl ether (50 cc) and distilled water (15 cc). The organic phase is separated, dried over potassium carbonate and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residual viscous yellow oil is purified by chromatography on a column (height: 35 cm; diameter: 2.6 cm) of silica gel (0.2-0.063 mm), eluting with ethyl acetate (300 cc) and collecting 25-cc fractions. Fractions 3 to 9 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. N-Pentyl-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide (2.25 g) is thereby obtained in the form of a yellow oil. 0.55 g of this product is dissolved in isopropyl ether (20 cc), and a 3.3N solution (0.6 cc) of hydrochloric acid in isopropyl ether is introduced dropwise and with stirring. The precipitate formed is drained, washed with isopropyl ether (3×5 cc) and dried under reduced pressure (5 mm Hg; 0.68 kPa) at 40° C. N-Pentyl-10-[(2RS)-1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide hydrochloride (0.56 g) is thereby obtained in the form of a pale yellow powder, m.p. 155°-160° C. (melts forming a paste).

1. temperatureAfter cooling
2. concentrationthe mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
3. distillationdistilled water (15 cc)
4. customThe organic phase is separated
5. dry with materialdried over potassium carbonate
6. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
7. customThe residual viscous yellow oil is purified by chromatography on a column (height: 35 cm; diameter: 2.6 cm) of silica gel (0.2-0.063 mm)
8. washeluting with ethyl acetate (300 cc)
9. customcollecting 25-cc fractions
10. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C