反应详情

温度

50 °C

Well-dried magnesium (8.3 g) and THF (20 ml) were put in a reaction vessel under a nitrogen atmosphere, and heated to 50° C. 1-Bromo-3-fluorobenzene (14) (60.0 g) dissolved in THF (300 ml) was slowly added dropwise thereto in the temperature range of 40° C. to 60° C., and the mixture was stirred for another 60 minutes. Then, 1,4-dioxaspiro[4.5]decan-8-one (15) (64.3 g) dissolved in THF (150 ml) was slowly added dropwise thereto in the temperature range of 50° C. to 60° C., and the mixture was stirred for another 60 minutes. The reaction mixture was cooled to 30° C., and then poured into a vessel containing an aqueous 1N—HCl solution (900 ml) and ethyl acetate (500 ml), and mixed. The mixture was then allowed to stand until it had separated into two phases, the organic and aqueous phases, and an extractive operation to an organic phase was carried out. The organic phase was fractionated, and washed sequentially with water and a saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure, giving 74.6 g of 8-(3-fluorophenyl)-1,4-dioxaspiro[4,5]decan-8-ol (16).

1. additionwas slowly added dropwise
2. additionwas slowly added dropwise
3. stirringin the temperature range of 50° C. to 60° C., and the mixture was stirred for another 60 minutes
4. temperatureThe reaction mixture was cooled to 30° C.
5. additionpoured into a vessel
6. additionmixed
7. customhad separated into two phases
8. washwashed sequentially with water
9. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and then dried over anhydrous magnesium sulfate
10. distillationThe solvent was then distilled off under reduced pressure