反应详情

A solution of 7-chloro-3-(aminocarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (590 mg, 2.03 mmol) (compound of Example 14) in phosphorous oxychloride (2.56 mL) was refluxed for 70 minutes. The excess phosphorous oxychloride was distilled off at atmospheric pressure and 106° C. To the remaining dark brown residue was added water (40 mL). The aqueous phase was extracted with ethyl acetate (4×50 mL). The organic layers were combined and dried over magnesium sulfate, filtered, and concentrated on a rotary evaporator to give the title compound as a brown/gold solid (≈216 mg, 39% yield, m.p. 370° C. dec.).

1. distillationThe excess phosphorous oxychloride was distilled off at atmospheric pressure and 106° C
2. additionTo the remaining dark brown residue was added water (40 mL)
3. extractionThe aqueous phase was extracted with ethyl acetate (4×50 mL)
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated on a rotary evaporator