反应详情

温度

53 °C

Seventh Step: 1.76 g of well dried magnesium and 10 mL of THF were placed in a reactor under nitrogen atmosphere, and heated to 53° C. 17.2 g of the compound (1) dissolved in 30 mL of THF was slowly added dropwise thereto at a temperature range of from 50 to 56° C., followed by stirring for 30 minutes. Thereafter, 6.0 g of the compound (16) dissolved in 10 mL of THF was slowly added dropwise thereto at a temperature range of from 50 to 55° C., followed by stirring for 30 minutes. After cooling the resulting reaction mixture to 25° C., the reaction mixture was poured into and mixed with a mixture of 100 mL of 1N hydrochloric acid and 100 mL of toluene. The mixture was then separated into an organic layer and an aqueous layer by standing still, so as to attain extraction to the organic layer. The resulting organic layer was fractionated and washed with water, a 2N sodium hydroxide aqueous solution, a saturated sodium bicarbonate aqueous solution, and water, followed by drying over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure to obtain 18.5 g of 1-(4-ethoxy-2,3-difluorophenyl)-4-vinylcyclohexanol (17) as a yellow liquid.

1. additionwas slowly added dropwise
2. customof from 50 to 56° C.
3. additionwas slowly added dropwise
4. customof from 50 to 55° C.
5. stirringby stirring for 30 minutes
6. temperatureAfter cooling
7. customthe resulting reaction mixture to 25° C.
8. additionthe reaction mixture was poured into and
9. customThe mixture was then separated into an organic layer
10. extractionextraction to the organic layer
11. washwashed with water
12. dry with materialby drying over anhydrous magnesium sulfate
13. customThereafter, the solvent was removed by distillation under reduced pressure