反应详情

To N,N-dimethylformamide (6 mL) solution of 2-(4-bromophenyl)ethanol (552 mg), imidazole (248 mg) and tert-butyldimethylsilyl chloride (453 mg) were added. The reaction solution was stirred at room temperature for 3 hours. To the reaction solution, 1N-hydrochloric acid (10 mL) was added. The aqueous layer was extracted twice with ethyl acetate. The combined organic layer was washed with water and saturated brine and then dried over anhydrous magnesium sulfate. After removing the anhydrous magnesium sulfate by filtration, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0→97:3) to obtain the title compound (829 mg) having the following physical properties.

1. extractionThe aqueous layer was extracted twice with ethyl acetate
2. washThe combined organic layer was washed with water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customAfter removing the anhydrous magnesium sulfate
5. filtrationby filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0→97:3)