反应详情

温度

100 °C

A solution of 10-[(2RS)-1-(N-ethyl-N-methyl-amino)-2-propyl]-2-phenothiazinecarbothioamide (1 g) and 3-methylbutylamine (4.9 cc) in absolute ethanol (15 cc) is saturated with hydrogen sulphide and heated for 16 hours to a temperature in the region of 100° C. After being cooled, the orange solution obtained is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residual orange oil is purified by chromatography on a column (height: 25 cm; diameter 2 cm) of silica gel (0.04-0.063 mm) under a slight excess pressure of nitrogen (40 kPa), eluting with a mixture (80:20 by volume) (500 cc) of ethyl acetate and cyclohexane and collecting 30-cc fractions. Fractions 4 to 8 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. N-(3-Methylbutyl)-10-[(2RS)-1-(N-ethyl-N-methylamino)-2-propyl]-2-phenothiazinecarbothioamide (1.3 g) is thereby obtained in the form of an orange-yellow oil.

1. temperatureAfter being cooled
2. customthe orange solution obtained
3. concentrationis concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
4. customThe residual orange oil is purified by chromatography on a column (height: 25 cm; diameter 2 cm) of silica gel (0.04-0.063 mm) under a slight excess pressure of nitrogen (40 kPa)
5. washeluting with a mixture (80:20 by volume) (500 cc) of ethyl acetate and cyclohexane
6. customcollecting 30-cc fractions
7. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C