反应详情

The (2β,3α,5α)-3-hydroxy-2-(2,2-dimethyl-4-morpholinyl)pregnane-11,20-dione (8.0 g), 2-aminoethanol (40 ml), toluene (200 ml) and Dowex 50-W resin (0.8 g) were added to a flask fitted with a water separator. The mixture was heated under reflux for 10 h, by which time approximately 15 ml of a distillate had collected in the water separator. The contents of the flask were filtered while still hot and the residue was rinsed with hot toluene. The filtrate was washed with water, dried over sodium sulfate and the solvent was removed under reduced pressure to give (2β,3α,5α)-3-hydroxy-20-[(2-hydroxyethyl)imino]-2-(2,2-dimethyl-4-morpholinyl)pregnan-11-one. δ (CDCl3) 0.50 (s,3H), 1.05 (s,3H), 1.21 (s,3H), 1.23 (s,3H) and 2.36 (s,2H).

1. temperatureThe mixture was heated
2. temperatureunder reflux for 10 h, by which time approximately 15 ml of a distillate
3. customhad collected in the water separator
4. filtrationThe contents of the flask were filtered while still hot and the residue
5. washwas rinsed with hot toluene
6. washThe filtrate was washed with water
7. dry with materialdried over sodium sulfate
8. customthe solvent was removed under reduced pressure