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
Paratoluenesulfonic acid (20 ml) was added to a solution of 235 mg of 1,1-(ethylenedioxy)-3-(10-hydroxydecyl)-4-methyl-3-(phenylsulfonyl)-cyclohexane in 20 ml of chloroform and 4 ml of acetone. The resulting mixture was reacted at 50° C. for 24 hours. To the reaction mixture were added 10 ml of a saturated aqueous solution of sodium bicarbonate, followed by extraction with dichloromethane. The organic layer was washed with saturated saline and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by chromatography on a silica gel column while using hexane-ethyl acetate, whereby 3-(10-hydroxydecyl)-4-methyl-2-cyclohexene-1-one was obtained in the form of a colorless oil. Yield: 75%, CCM: (hexane-AcOEt: 6-4) Rf=0.2
WORKUP
后处理
- customThe resulting mixture was reacted at 50° C. for 24 hours
- extractionfollowed by extraction with dichloromethane
- washThe organic layer was washed with saturated saline
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customThe residue was purified by chromatography on a silica gel column