HRID232758
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
After dissolving 39.2 g of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstan-17-one in a mixture of 392 ml of methanol and 56 ml of methylene chloride. 14.7 g Sodium borohydride are portionwise added while stirring and introducing nitrogen at such a rate that the temperature reaches room temperature as a maximum. The solution containing a precipitate is left to stand for 12 hours, then methylene chloride is evaporated, and the residue is diluted with water. The precipitate is filtered, thoroughly washed with water, dried and recrystallized from methanol to obtain the title product in a yield of 33.3 g (89.5%), m.p.: 167°-169° C.
WORKUP
后处理
- additionintroducing nitrogen at such a rate that the temperature
- customreaches room temperature as a maximum
- additionThe solution containing a precipitate
- waitis left
- custommethylene chloride is evaporated
- additionthe residue is diluted with water
- filtrationThe precipitate is filtered
- washthoroughly washed with water
- customdried
- customrecrystallized from methanol