反应详情

温度

-20 °C

To a solution of 8 (71 mg, 0.2 mmol) in CH2Cl2 (5 mL) was added a 1M solution of boron tribromide (0.4 mL, 0.4 mmol) in CH2Cl2 at −78° C. The solution was stirred for an additional 2 h and at −20° C. for 5 h then quenched with water (10 mL). The precipitate was collected by filtration and recrystallized from CH2Cl2 to afford crude product 5 (30 mg, 46%). 1H NMR (400 MHz, DMSO) δ 3.93 (s, 3H), 7.01 (s, 1H), 7.21 (s, 1H), 8.38-8.39 (m, 4H).

1. customthen quenched with water (10 mL)
2. filtrationThe precipitate was collected by filtration
3. customrecrystallized from CH2Cl2