反应详情

To a solution of 5.0 g of 3β-acetoxy-14β-hydroxy-17β-methyl-5β-androstane (VIII-a) in pyridine (100 mL), 3.5 g of thionyl chloride were added at 0° C. The solution was stirred at the same temperature for 2.5 hrs and then poured in 100 mL of 1N HCl and crushed ice: the mixture was extracted with ethyl ether: the organic layer was washed with a saturated aqueous solution of disodium hydrogen phosphate, dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure to give 4.5 g of 3β-acetoxy-17β-methyl-5β-androst-14-ene as a white solid.

1. customcrushed ice
2. extractionthe mixture was extracted with ethyl ether
3. washthe organic layer was washed with a saturated aqueous solution of disodium hydrogen phosphate
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated to dryness under reduced pressure