反应详情

Aluminium (3.64 g, 0.089 mol), leadbromide (2.23 g, 0.0089 mol) and 36% HCl (15.13 ml, 0.178 mol) were added to 200 ml of methanol, the mixture was stirred, and 2-chloro-4-(2,2,2-trichloro-1-hydroxyethyl)phenol (24.55 g, 0.089 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 column chromatography (ethyl acetate:n-hexane=1:4) to obtain the title compound (17.3 g, 87%).

1. stirringThe mixture was stirred at 60° C. for 4 hours
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