反应详情

A solution of 5-bromo-2,2-difluorobenzodioxole (1.18 g, 4.97 mmol) in anhydrous diethyl ether (8 mL) at −78° C. was treated with 2.5M n-BuLi in hexane (2.4 mL, 5.97 mmol), stirred for 1 hour, and treated with triisopropyl borate (1.5 mL, 6.46 mmol). The mixture was slowly warmed to room temperature and stirred for about 18 hours. The reaction was quenched with saturated NH4Cl/10% HCl and extracted with ethyl acetate. The combined extracts were dried (MgSO4), filtered, and concentrated. The concentrate was used directly without further purification. 1H NMR (CD3OD) δ 7.26-7.11 (m, 3H).

1. stirringstirred for about 18 hours
2. customThe reaction was quenched with saturated NH4Cl/10% HCl
3. extractionextracted with ethyl acetate
4. dry with materialThe combined extracts were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe concentrate was used directly without further purification