反应详情

With stirring, imidazole (1.1 g, 16.0 mmol) is added to a solution of 3,5-dibromobenzyl alcohol (2.8 g, 10.5 mmol) in absolute DMF (20 ml), and the mixture is cooled to 0° C. tert-Butyldiphenylsilyl chloride (3.3 ml, 17.8 mmol) is added dropwise to the reaction solution, which is then stirred at 0° C. for 2 h. The mixture is then warmed to RT and stirred for another 2 h. The reaction mixture is diluted with ethyl acetate (20 ml) and extracted with a semisaturated aqueous NH4Cl solution (20 ml). The organic phase is dried over MgSO4, filtered off and concentrated under reduced pressure. Further purification is carried out by chromatography [PE/EA (99:1)] on a silica gel column. This gives the title compound (5.0 g) as a colorless solid. TLC, silica gel (glass plates), [petroleum ether/ethyl acetate (99:1)], Rf=0.8.

1. additionis added dropwise to the reaction solution, which
2. stirringis then stirred at 0° C. for 2 h
3. stirringstirred for another 2 h
4. extractionextracted with a semisaturated aqueous NH4Cl solution (20 ml)
5. dry with materialThe organic phase is dried over MgSO4
6. filtrationfiltered off
7. concentrationconcentrated under reduced pressure
8. customFurther purification