反应详情

温度

60 °C

Aluminum (3.73 g, 0.091 mol), lead bromide (2.28 g, 0.0091 mol) and 36% HC (15.47 ml, 0.182 mol) were added to 200 ml of methanol, and 3-(2,2,2-trichloro-1-hydroxyethyl)phenol (12.57 g, 0.091 mol) obtained in Step 1 was added thereto. The mixture was stirred at 60° C. for 4 hours. The solvent was removed therefrom under a reduced pressure. Ice was added to the reaction mixture and resulting mixture was washed three times with n-hexane and ether (1:1). The organic layer was dried over anhydrous magnesium sulfate, filtered and distilled under a reduced pressure. The resulting residue was subjected to silica gel column chromatography (ethyl acetate:n-hexane=1:9) to obtain the title compound (16.0 g, 93%).

1. additionwas added
2. customThe solvent was removed
3. additionIce was added to the reaction mixture
4. customresulting mixture
5. washwas washed three times with n-hexane and ether (1:1)
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. filtrationfiltered
8. distillationdistilled under a reduced pressure