反应详情

A mixture of Example 103B (20 mg, 0.055 mmol), NaCNBH3 (17.2 mg, 0.275 mmol), and ammonium acetate (42 mg, 0.55 mmol) in methanol (5 mL) was heated to reflux overnight and concentrated. The concentrate was purified by reverse-phase HPLC to provide the desired product. MS (ESI) m/e 363 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 8.4 (br s, 2H), 7.66 (m, 2H), 7.36 (m, 2H), 7.25 (d, 1H), 7.14 (d, 1H), 4.42 (br s, 1H), 2.65 (m, 2H), 2.06 (m, 2H), 1.68 (m, 2H).

1. temperatureto reflux overnight
2. concentrationconcentrated
3. customThe concentrate was purified by reverse-phase HPLC