반응 #310616
ord-45054b6002454d509711c87a55c276dc
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후처리
- 1추출the mixture was extracted with ether (x2)
- 2세척The extract was washed with water (x2)
- 3기타dried
- 4기타evaporated
- 5기타to leave a froth which
- 6세척the mixture was washed with ether (x2)
- 7추출The wash was extracted with 2M-HCl solution
- 8추출The mixture was extracted with ether (x2)
- 9세척the extract was washed with water (x2)
- 10기타dried
- 11기타evaporated
- 12기타to leave a froth which
- 13기타was purified by column chromatography
- 14세척eluted with CHCl3 :MeOH (9:1)
실험 절차
A solution of 11α-amino-2β-ethoxy-3α-hydroxy-5α-pregnan-20-one 20-ethylene acetal (2 g) in ethanol (20 ml) was stirred with cyclohexanone (1.5 ml) and sodium cyanoborohydride (2.015 g) for 6 h. 5% NaHCO3 solution (40 ml) was added and the mixture was extracted with ether (x2). The extract was washed with water (x2), dried and evaporated to leave a froth which was dissolved in 2M-HCl solution (50 ml) and ethanol (50 ml). Water (100 ml) was added and the mixture was washed with ether (x2). The wash was extracted with 2M-HCl solution and the combined acid fraction was brought to basic pH with 2M-NaOH solution. The mixture was extracted with ether (x2) and the extract was washed with water (x2), dried and evaporated to leave a froth which was purified by column chromatography eluted with CHCl3 :MeOH (9:1) to give the title compound (1.235 g), [α]D +39°. νmax 1695 cm-1.