反应详情

温度

140 °C

1,2-Diaminocyclohexane (7.98 g) is added to an ethanolic solution (32 cc) of 10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarbothioamide, L series (2.96 g). The mixture is heated in an autoclave to 140° C. for 18 hours, then diluted with ethyl acetate (150 cc) and washed with distilled water (3×50 cc). The organic phase is separated after settling has taken place, dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residue is purified by chromatography on a column (height: 24 cm; diameter: 2.5 cm) of neutral alumina, eluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 75:25 (500 cc), 50:50 (750 cc) and 25:75 (750 cc) and collecting 50-cc fractions. Fractions 10 to 29 containing the pure product are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give 2-(3a, 4, 5, 6, 7, 7a-hexahydro-1H-benzimidazol-2-yl)-10-[1-(1-pyrrolidinyl)-2-propyl]phenothiazine, L series (0.38 g) in the form of a brown product of meringue-like consistency.

1. washwashed with distilled water (3×50 cc)
2. customThe organic phase is separated after settling
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
6. customThe residue is purified by chromatography on a column (height: 24 cm; diameter: 2.5 cm) of neutral alumina
7. washeluting with mixtures of cyclohexane and ethyl acetate in proportions (by volume) of 75:25 (500 cc), 50:50 (750 cc) and 25:75 (750 cc)
8. customcollecting 50-cc fractions
9. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.