反应详情

At 0° C., 16.23 g (71.75 mmol) of 8-(trifluoromethyl)-1,4-dioxaspiro[4.5]decan-8-ol (Example 7A) were dissolved in 582 ml of tetrahydrofuran, 5.74 g (143.50 mmol) of sodium hydride (60% in paraffin oil) were added a little at a time and the mixture was stirred at room temperature for 1 hour. 50.92 g (358.76 mmol) of iodomethane were added dropwise to the resulting suspension, and the reaction mixture was stirred at room temperature overnight. For work-up, the mixture was poured into about 1 l of ice-water and the product was extracted with dichloromethane. The organic phase was washed repeatedly with water, dried over sodium sulphate and concentrated under reduced pressure. Drying gave 17.34 g (100% of theory) of the title compound as a brownish oil.

1. stirringthe reaction mixture was stirred at room temperature overnight
2. extractionthe product was extracted with dichloromethane
3. washThe organic phase was washed repeatedly with water
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customDrying