反应详情

温度

25 °C

A solution of mercuric acetate (0.84 g) in glacial acetic acid (13 cc) is added dropwise during a period of 10 minutes to a solution of 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarbothioamide (1.12 g) in glacial acetic acid (13 cc). The reaction mixture is stirred for 90 minutes at 25° C. and then filtered on sintered glass covered with celite. The celite is washed with acetic acid (2 cc) and the combined filtrates are concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give a residue which is then diluted in ethyl acetate (50 cc). The organic phase is washed with normal caustic soda solution (25 cc) and distilled water (3×25 cc) and then with brine (1×25 cc), dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give a residue which is purified by chromatography on a column (height: 17.2 cm; diameter: 2.4 cm) of silica gel (0.04-0.06 mm) with a slight excess pressure of nitrogen (40 kPa), eluting with a 50:50 (by volume) mixture (1 liter) of cyclohexane and ethylacetate, collecting 60-cc fractions. Fractions 4 to 14 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide (0.83 g).

1. filtrationfiltered on sintered glass
2. washThe celite is washed with acetic acid (2 cc)
3. concentrationthe combined filtrates are concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
4. customto give a residue which
5. washThe organic phase is washed with normal caustic soda solution (25 cc)
6. distillationdistilled water (3×25 cc)
7. dry with materialwith brine (1×25 cc), dried over magnesium sulphate
8. filtrationfiltered
9. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
10. customto give a residue which
11. customis purified by chromatography on a column (height: 17.2 cm; diameter: 2.4 cm) of silica gel (0.04-0.06 mm) with a slight excess pressure of nitrogen (40 kPa)
12. washeluting with a 50:50 (by volume) mixture (1 liter) of cyclohexane and ethylacetate
13. customcollecting 60-cc fractions
14. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.