反应详情

A solution of 2-(3-bromobenzyloxy)ethanol [Aromatic Intermediate 25, step a] (3 g), imidazole (2.2 g) and tert-butyldimethylchlorosilane (2.2 g) in DCM (50 mL) was stirred at RT for 17 hours. The reaction mixture was partitioned between ethyl acetate and water. The aqueous layer was extracted with ethyl acetate (×2). The combined organic phases were dried and evaporated in vacuo. The crude product was purified by silica gel chromatography, gradient elution 10 to 40% ethyl acetate in isohexane. Fractions containing the product were evaporated to dryness to afford the subtitled compound as a colourless oil. Yield 3.8 g.

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. extractionThe aqueous layer was extracted with ethyl acetate (×2)
3. customThe combined organic phases were dried
4. customevaporated in vacuo
5. customThe crude product was purified by silica gel chromatography, gradient elution 10 to 40% ethyl acetate in isohexane
6. additionFractions containing the product
7. customwere evaporated to dryness