反应详情

Potassium thioacetate (1.32 g) was added to a solution of the 21-chloro-compound of Example 2 (2.22 g) in ethanol (11.1 ml). The mixture was heated under reflux in an atmosphere of nitrogen for 40 min and then poured into water (100 ml). The precipitated solid was filtered off, washed with water and dissolved in dichloromethane. After drying the solution over sodium sulfate the solvent was removed under reduced pressure and the residue was chromatographed on silica gel. The purified product was crystallised from methanol to give (2β,3α,5α)-21-(acetylthio)-3-hydroxy-2-(2,2-dimethyl-4-morpholinyl)pregnane-11,20-dione (1.46 g). m.p. 181°-182° C.; [α]D +131.9° (c 0.88).

1. temperatureThe mixture was heated
2. temperatureunder reflux in an atmosphere of nitrogen for 40 min
3. filtrationThe precipitated solid was filtered off
4. washwashed with water
5. dissolutiondissolved in dichloromethane
6. dry with materialAfter drying the solution over sodium sulfate the solvent
7. customwas removed under reduced pressure
8. customthe residue was chromatographed on silica gel
9. customThe purified product was crystallised from methanol