HRID1077008
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
Propane-2-thiol (1.3 ml.) was added to a warm solution of sodium (0.6 g.) in a mixture of propan-2-ol (25 ml.) and toluene (30 ml.). 21-Bromo-3α-hydroxy-5α-pregnane-11,20 -dione (0.7 g.) was then added and the mixture was gently refluxed for 2 hr. The mixture was then partitioned between water and ether and the organic layer was washed with water, dried (Na2SO4) and evaporated. The residual foam was purified by preparative t.l.c. (CHCl3) to give title compound (0.2 g.) as a white foam, [α]D + 67° (c 1.3).
WORKUP
后处理
- temperaturethe mixture was gently refluxed for 2 hr
- customThe mixture was then partitioned between water and ether
- washthe organic layer was washed with water
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residual foam was purified by preparative t.l.c