反应详情

温度

100 °C

A solution of D series 2-(2-cyano-10-phenothiazinyl)-propyl methanesulphonate (6.8 g) in toluene (80 cc) and (2RS)-2-methylpyrrolidine (3.5 cc) is heated with stirring at 100° C. for 48 hours. After cooling to 25° C., the mixture is transferred into a separating funnel where it is washed with distilled water (2×200 cc) and brine (50 cc). The organic phase is dried over magnesium sulphate and filtered, and the filtrate is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) to give a residue which is purified by chromatography on a column (height: 35 cm; diameter: 3.2 cm) of silica (0.2-0.06 mm), eluting with a mixture of cyclohexane and ethyl acetate 70-30 (by volume) (1 liter), collecting fractions of 60 cc. Fractions 11 to 14 are pooled and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) to give 10-{1-[(2RS)-2-methyl-1-pyrrolidinyl]-2-propyl}-2-phenothiazinecarbonitrile, D series (0.5 g), in the form of a yellow oil.

1. temperatureAfter cooling to 25° C.
2. customthe mixture is transferred into a separating funnel
3. washwhere it is washed with distilled water (2×200 cc) and brine (50 cc)
4. dry with materialThe organic phase is dried over magnesium sulphate
5. filtrationfiltered
6. concentrationthe filtrate is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa)
7. customto give a residue which
8. customis purified by chromatography on a column (height: 35 cm; diameter: 3.2 cm) of silica (0.2-0.06 mm)
9. washeluting with a mixture of cyclohexane and ethyl acetate 70-30 (by volume) (1 liter)
10. customcollecting fractions of 60 cc
11. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa)