反应详情

3-Methylbutylamine (10.7 cc) is added to a solution of 10-(1-diethylamino-2-propyl)-2-phenothiazinecarbothioamide acid fumarate, L series (3 g), in absolute ethanol (45 cc) and this solution is saturated with hydrogen sulphide. The mixture is then brought to a temperature in the region of 105° C. for 16 hours and concentrated to dryness under reduced pressure (30 mm Hg; 4 pKa). The residual orange-colored oil is purified by chromatography on a column (height: 35 cm; diameter: 3 cm) of silica gel (0.2-0.063 mm), eluting with mixture (400 cc) of ethyl acetate and cyclohexane (70:30 by volume) and collecting 30-cc fractions. Fractions 7 to 11 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 pKa) at 50° C. to give 10-(1-diethylamino-2-propyl)-N-(3-methyl-1-butyl)-2-phenothiazinecarbothioamide, L series (3.1 g), in the form of an orange-colored oil.

1. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 pKa)
2. customThe residual orange-colored oil is purified by chromatography on a column (height: 35 cm; diameter: 3 cm) of silica gel (0.2-0.063 mm)
3. washeluting with mixture (400 cc) of ethyl acetate and cyclohexane (70:30 by volume)
4. customcollecting 30-cc fractions
5. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 pKa) at 50° C.