反应详情

Into 7.6 g of magnesium and 20 mL of THF which were stirred while water-cooling in a nitrogen atmosphere, a THF solution (200 mL) containing 60 g of 2,3,4-trifluorobromobenzene was added dropwise for 2 hours, and stirred for 3 hours. Into this, a THF solution (200 mL) containing 70 g of 4-(trans-4-propylcyclohexyl)cyclohexanone was added dropwise for 2 hours, and stirred for 2 hours. After the reaction solution was poured into 10% hydrochloric acid and stirred for a while, an organic layer was separated, and an aqueous layer was extracted with toluene. After the extract and the organic layer were mixed together, washed using water and a saturated saline solution in that order, and dried using anhydrous sodium sulfate, the solvent was evaporated under a reduced pressure to obtain 110 g of 2,3,4-trifluoro-1-[1-hydroxy-4-(trans-4-propylcyclohexyl)cyclohexyl]benzene (unsatisfactorily dried).

1. temperaturecooling in a nitrogen atmosphere
2. additionwas added dropwise for 2 hours
3. additionwas added dropwise for 2 hours
4. stirringstirred for 2 hours
5. stirringstirred for a while
6. customan organic layer was separated
7. extractionan aqueous layer was extracted with toluene
8. extractionAfter the extract
9. additionthe organic layer were mixed together
10. washwashed
11. customa saturated saline solution in that order, and dried
12. customthe solvent was evaporated under a reduced pressure