反应详情

温度

0 °C

In 20 ml of pyridine was dissolved 0.58 g of the 1α,3β-bis(tetrahydropyran-2-yloxy)cholesta-5,7-dien-22-ol obtained as above. To this solution was added 0.12 g of methanesulfonyl chloride and the mixture was stirred at 0° C. for 2 hours. Then, at room temperature, the reaction mixture was diluted with water and extracted with diethyl ether. The extract was washed with water and dried over anhydrous sodium sulfate. The low-boiling fraction was then distilled off under reduced pressure and the residue was purified by silica gel column chromatography. The procedure yielded 0.57 g of 1α,3β-bis(tetrahydropyran-2-yloxy)cholesta-5,7-dien-22-yl methanesulfonate (yield: 86%).

1. customobtained as above
2. extractionextracted with diethyl ether
3. washThe extract was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe low-boiling fraction was then distilled off under reduced pressure
6. customthe residue was purified by silica gel column chromatography