反应详情

Triethylamine (98.4 cc) is added to a solution of 10-[(1RS)-2-hydroxy-1-methylethyl]-2-phenothiazine-carbonitrile (197.7 g) in anhydrous pyridine (750 cc), and hydrogen sulphide is bubbled through for 6 hours 30 minutes at 25° C. while the mixture is kept stirred. The mixture is stirred for 16 hours at 25° C., then purged with a stream of nitrogen for 2 hours and poured into distilled water (3000 cc). The oil which forms is separated after settling has taken place, washed with distilled water (3×1000 cc) and dissolved in ethyl acetate (3000 cc). The solution obtained is washed with distilled water (7×1 liter), dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give a yellow crystalline mass (225 g). This product is recrystallized in ethanol (1350 cc) to give 10-[(1RS)-2-hydroxy-1 -methylethyl]-2-phenothiazinecarbothioamide (158.4 g) in the form of yellow crystals, m.p. 152° C.

1. customis bubbled through for 6 hours 30 minutes at 25° C. while the mixture
2. stirringThe mixture is stirred for 16 hours at 25° C.
3. custompurged with a stream of nitrogen for 2 hours
4. additionpoured
5. distillationinto distilled water (3000 cc)
6. customThe oil which forms is separated after settling
7. washwashed with distilled water (3×1000 cc)
8. dissolutiondissolved in ethyl acetate (3000 cc)
9. customThe solution obtained
10. washis washed with distilled water (7×1 liter)
11. dry with materialdried over magnesium sulphate
12. filtrationfiltered
13. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
14. customto give a yellow crystalline mass (225 g)
15. customThis product is recrystallized in ethanol (1350 cc)