反应详情

n-Butylamine (2.4 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 40° C. The residue obtained is purified by chromatography on a column (height: 17 cm; diameter: 2.6 cm) of silica gel (0.04-0.06 mm) with a slight excess pressure of nitrogen (40 kPa), eluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 90:10 (250 cc), 80:20 (500 cc) and 50:50 (750 cc) and then with pure ethyl acetate (750 cc), collecting 50-cc fractions. Fractions 10 to 18 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give N-butyl-10-[(2RS)-1-diethylamino-2-propyl]-2-phenothiazinecarbothioamide (0.96 g).

1. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
2. customThe residue obtained
3. customis purified by chromatography on a column (height: 17 cm; diameter: 2.6 cm) of silica gel (0.04-0.06 mm) with a slight excess pressure of nitrogen (40 kPa)
4. washeluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 90:10 (250 cc), 80:20 (500 cc) and 50:50 (750 cc)
5. customwith pure ethyl acetate (750 cc), collecting 50-cc fractions
6. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.