HRID1077010
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
A solution of 21-bromo-3α-hydroxy-5α-pregnane-11,20-dione (0.75 g.) in acetone (50 ml.) was treated with a solution of barium thiocyanate (2.6 g.) in water (10 ml.). The resulting mixture was refluxed for 4 hr., cooled and then partitioned between water and ether. The organic layer was washed with water, dried (Na2SO4) and evaporated. The residue (720 mg.) was purified by preparative t.l.c. (EtOAc) to afford title compound (685 mg.) as a white foam, [α]D + 67°.
WORKUP
后处理
- temperatureThe resulting mixture was refluxed for 4 hr
- temperature, cooled
- custompartitioned between water and ether
- washThe organic layer was washed with water
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue (720 mg.) was purified by preparative t.l.c