反应详情

温度

120 °C

To a stirred solution of Example 1 (200 mg, 0.5 mmol) in ethoxyethanol (5 mL) was added hydrazine hydrate (1.5 mmol). The reaction mixture was heated to 120° C. for 6 h. Upon cooling the reaction mixture was poured into sat NaHCO3 aq and extracted with DCM (×2). The combined organic fractions were dried (MgSO4) and concentrated in vacuo. Purification by flash column chromatography (silica, 5% EtOH in DCM) gave the title compound (86 mg, 46%). δH (CDCl3) 8.76 (1H, br s), 8.60 (1H, br s), 7.55-7.7 (3H, m), 7.4-7.5 (2H, m), 7.25-7.35 (3H, m), 6.9-7.0 (2H, m), 6.35 (1H, d, J 10 Hz), 4.3 (2H, br s). LCMS (ES+) RT 2.84 minutes, 377 (M+H)+.

1. temperatureUpon cooling the reaction mixture
2. additionwas poured
3. extractionextracted with DCM (×2)
4. dry with materialThe combined organic fractions were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customPurification by flash column chromatography (silica, 5% EtOH in DCM)