反应详情

温度

90 °C

In a 100 mL round-bottom flask a mixture of methyl 4-hydroxy-9H-pyrimido[4,5-b]indole-7-carboxylate (1.1 g, 4.5 mmol) and phosphorous oxychloride (15 mL, 161 mmol) was heated to 90° C. for 16 hours, cooled down to room temperature and evaporated under reduced pressure. The residue was suspended in dichloromethane (20 mL) and filtered through Celite. Evaporation afforded the title compound as an orange solid (360 mg). LCMS m/z 262.0 (M+H)+, retention time (on analytical HPLC)=2.02 minutes.

1. temperaturecooled down to room temperature
2. customevaporated under reduced pressure
3. filtrationfiltered through Celite
4. customEvaporation