反应详情

温度

40 °C

1.5 g of well dried magnesium and 30 mL of THF were placed in a reactor under nitrogen atmosphere, and heated to 40° C. 15.3 g of the compound (1) dissolved in 30 mL of THF was slowly added dropwise thereto at a temperature range of from 35 to 49° C., followed by stirring for 30 minutes. Thereafter, 5.0 g of the compound (23) dissolved in 5 mL of THF was slowly added dropwise thereto at a temperature range of from 30 to 40° 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 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 16.0 g of 1-(3-chloro-4-ethoxy-2-fluorophenyl)-4-vinylcyclohexanol (24) as a yellow liquid.

1. additionwas slowly added dropwise
2. customof from 35 to 49° C.
3. additionwas slowly added dropwise
4. customof from 30 to 40° 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 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