反应详情

A solution of 109 (270 mg, 0.6 mmol) in dichloromethane (20 mL) was treated with BCl3 (6 mL, 6 mmol, 1M in dichloromethane) for 2 hours at −60° C., then the reaction was quenched with methanol (20 mL). Volatiles were distilled out under vacuum to give a residue, which was dissolved into methanol (5 mL) and neutralized by Con. NH4OH (2 ml, 26% aqueous solution). After concentration, the crude product was purified by a silica gel column, eluted with 10% methanol in dichloromethane to give the title compound as a white solid (41 mg, 25%); (ES, m/z) [M+H]+ 283.0; 1HNMR (300 MHz, D2O) δ 6.17 (d, J=6.3 Hz, 1H), 5.77-6.14 (m, 1H), 4.12 (t, J=6.0 Hz, 1H), 3.93 (t, J=5.1 Hz, 1H), 3.68-3.73 (m, 1H), 3.43-3.48 (m, 1H), 2.91 (s, 6H), 1.99-2.35 (m, 2H).

1. customthe reaction was quenched with methanol (20 mL)
2. distillationVolatiles were distilled out under vacuum
3. customto give a residue, which
4. concentrationAfter concentration
5. customthe crude product was purified by a silica gel column
6. washeluted with 10% methanol in dichloromethane