反应详情

Isobutylamine (2.50 cc) is added to a solution of 10-[(2RS)-1-diethylamino-2-propyl]-2-phenothiazinecarbothioamide (1.86 g) in absolute ethanol (25 cc). The mixture is brought to 150° C. for 16 hours and then concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C. The residue obtained is purified by chromatography on a column (height: 16.5 cm; diameter: 2.8 cm) silica gel (0.04-0.06 mm) with a slight excess presof sure of nitrogen (40 kPa), eluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 80:20 (1.5 liters) and 50:50 (1 liter), collecting 50-cc fractions. Fractions 4 to 15 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarbothioamide (1.3 g).

1. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C
2. customThe residue obtained
3. customis purified by chromatography on a column (height: 16.5 cm; diameter: 2.8 cm) silica gel (0.04-0.06 mm) with a slight excess presof sure of nitrogen (40 kPa)
4. washeluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 80:20 (1.5 liters) and 50:50 (1 liter)
5. customcollecting 50-cc fractions
6. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.