反应详情

Phosphorus oxychloride (2 mL) was added to the 5-oxo-5,6-dihydrobenzo[c][2,6]naphthyridine-8-carbonitrile (150 mg, 0.66 mmol). The mixture was heated reflux for 3 hours at which time LCMS analysis indicated the absence of any starting material. Volatiles were removed under vacuum and the crude product was dissolved in dichloromethane, washed with brine and saturated aqueous sodium bicarbonate and dried over sodium sulfate. After concentrating under vacuum, the crude product was triturated with ethyl acetate and hexanes to give 5-chlorobenzo[c][2,6]naphthyridine-8-carbonitrile (125 mg). LCMS (ESI) 240.3 (M+1)+.

1. temperatureThe mixture was heated
2. temperaturereflux for 3 hours at which time LCMS analysis
3. customVolatiles were removed under vacuum
4. dissolutionthe crude product was dissolved in dichloromethane
5. washwashed with brine and saturated aqueous sodium bicarbonate
6. dry with materialdried over sodium sulfate
7. concentrationAfter concentrating under vacuum
8. customthe crude product was triturated with ethyl acetate and hexanes