反应详情

Methanesulfonyl chloride (0.23 ml, 2.93 mmol) was added dropwise, at room temperature, to a solution of alcohol (b) (0.5 g, 2.79 mmol) and triethylamine (0.41 ml, 3 mmol) in tetrahydrofuran (20 ml) and the mixture was stirred for 3 hours. More methane sulfonyl chloride (0.1 ml) and triethylamine (0.1 ml) were added and stirring was continued over night. The same amount of reagent was added yet again and stirring continued for 2 hours. The solvent was then concentrated, the residue was suspended in water and extracted with dichloromethane. The organic phase was dried over magnesium sulfate and concentrated. The solid residue was chromatographed on silica gel eluting with heptane-ethyl acetate (1-1) to give the product (0.2 g, 28%).

1. stirringstirring
2. waitwas continued over night
3. additionThe same amount of reagent was added yet again
4. stirringstirring
5. waitcontinued for 2 hours
6. concentrationThe solvent was then concentrated
7. extractionextracted with dichloromethane
8. dry with materialThe organic phase was dried over magnesium sulfate
9. concentrationconcentrated
10. customThe solid residue was chromatographed on silica gel eluting with heptane-ethyl acetate (1-1)