反应详情

温度

65 °C

Potassium acetate (0.83 g) was added to a solution of the 21-chloro compound of Example 2 (0.5 g), potassium iodide (0.04 g), glacial acetic acid (1.05 ml) and N,N-dimethylformamide (20 ml) and the mixture was heated at 65° C. in an atmosphere of nitrogen for 1.5 h. The mixture was then poured into water (200 ml) and aqueous sodium carbonate was added until the pH exceeded 9. The precipitated solid was filtered off, washed with water and dissolved in dichloromethane. After drying over sodium sulfate, the solvent was removed under reduced pressure and the residue was crystallised from methanol to give (2β,3α,5α)-21-(acetyloxy)-3-hydroxy-2-(2,2-dimethyl-4-morpholinyl)pregnane-11,20-dione (0.33 g). m.p. 158°-160° C.; [α]D +123° (c 0.68).

1. additionwas added until the pH
2. filtrationThe precipitated solid was filtered off
3. washwashed with water
4. dissolutiondissolved in dichloromethane
5. dry with materialAfter drying over sodium sulfate
6. customthe solvent was removed under reduced pressure
7. customthe residue was crystallised from methanol