反应详情

To 100 ml of tetrahydrofuran, 4.45 g (36 mmol) of 4,4-difluoro-3-methyl-3-butenol and 4.59 g (40 mmol) of methanesulfonyl chloride were dissolved, followed by drop-wisely adding 4.42 g (44 mmol) of triethylamine under ice-cooling. After the end of the drop-wise addition, the reaction liquid was stirred at room temperature for 1 hour. Hydrochloric acid salt of triethylamine was filtered, followed by adding water to the filtrate and extracting with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentrating under reduced pressure to obtain 7.20 g (yield: 99%) of 4,4-difluoro-3-methyl-3-butenyl methanesulfonate.

1. temperaturecooling
2. additionAfter the end of the drop-wise addition
3. customthe reaction liquid
4. filtrationHydrochloric acid salt of triethylamine was filtered
5. additionby adding water to the filtrate
6. extractionextracting with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materialby drying over anhydrous magnesium sulfate
9. concentrationconcentrating under reduced pressure