反应详情

tert-Butyldimethylsilyl chloride (9.03 g) was added portionwise to a stirred solution of 2-(4-fluorophenyl)ethanol (7 g) and imidazole (4.08 g) in DMF (100 mL) at 20° C. The reaction mixture was stirred for 3 hours at room temperature and then partitioned between ethyl acetate and brine. The organic layer was washed twice with brine, dried, filtered and the solvent concentrated under reduced pressure. The crude product was purified by flash silica chromatography eluting with 2% ethyl acetate in isohexane. Fractions containing the product were evaporated to dryness to afford the subtitled compound. Yield 11.60 g.

1. custompartitioned between ethyl acetate and brine
2. washThe organic layer was washed twice with brine
3. customdried
4. filtrationfiltered
5. concentrationthe solvent concentrated under reduced pressure
6. customThe crude product was purified by flash silica chromatography
7. washeluting with 2% ethyl acetate in isohexane
8. additionFractions containing the product
9. customwere evaporated to dryness