HRID559479
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
To cooled chlorosulfonic acid (16 ml, −10° C.) was cautiously added D7 (5 g, 0.024 mol) over a period of 2 h. Reaction was allowed to warm to ambient temperature and stirring continued for 3d. The reaction was then poured into ice-water slurry (500 ml), basified using solid potassium carbonate followed by extraction using DCM. Organic phase was separated, dried over MgSO4, filtered and concentrated under reduced pressure to leave an oil. Chromatography on silica gel eluting with ethyl acetate afforded the title compound as yellow oil.
WORKUP
后处理
- customof 2 h
- customReaction
- extractionfollowed by extraction
- customOrganic phase was separated
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto leave an oil