反应详情

3-(2-Chloroethyl)-8-methyl-4-oxo-(1H)-cinnoline (9 g, 0.04 mol) and phosphorus oxychloride (100 ml) were heated under reflux for 2 hours. The excess phosphorus oxychloride was evaporated under reduced pressure and the residue was poured onto ice, basified with concentrated ammonia solution and extracted with chloroform (3×200 ml). The chloroform extracts were combined, dried over magnesium sulphate, filtered and evaporated under reduced pressure to give a dark brown solid. Recrystallization from diethyl ether/petroleum ether (b.p. 40-60°) gave an analytically pure sample, m.p. 102-104°

1. temperatureunder reflux for 2 hours
2. customThe excess phosphorus oxychloride was evaporated under reduced pressure
3. additionthe residue was poured onto ice
4. extractionextracted with chloroform (3×200 ml)
5. dry with materialdried over magnesium sulphate
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customto give a dark brown solid
9. customRecrystallization from diethyl ether/petroleum ether (b.p. 40-60°)
10. customgave an analytically pure sample, m.p. 102-104°