反应详情

3-Methylbutylamine (12.9 cc) is added to a solution of 10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide, D series (4.1 g) in ethanol (61.5 cc), and the mixture is then saturated with hydrogen sulphide and heated for 16 hours to a temperature in the region of 105° C. After being cooled, the solution is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. A yellow oil is obtained, which is purified by chromatography on a column (height: 30 cc; diameter: 4 cm) of silica gel (0.2-0.063 mm), eluting with a mixture (95:5 by volume) (1.5 liters) of methylene chloride and methanol and collecting 80-cc fractions. Fractions 14 to 17 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. N-(3-Methylbutyl)-10-[1-(1-pyrrolidinyl)-2-propyl]-2phenothiazinecarbothioamide, D series (4.7 g) is obtained in the form of an orange oil.

1. temperatureAfter being cooled
2. concentrationthe solution is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
3. customA yellow oil is obtained
4. customwhich is purified by chromatography on a column (height: 30 cc; diameter: 4 cm) of silica gel (0.2-0.063 mm)
5. washeluting with a mixture (95:5 by volume) (1.5 liters) of methylene chloride and methanol
6. customcollecting 80-cc fractions
7. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C