反应详情

3-(2-Chloroethyl)-4-chloro-8-methylcinnoline (2.5 g, 0.01mol) and o-toluidine hydrochloride (1.4 g, 0.01 mol) in 1,4 dioxan (20 ml) were heated under reflux for 20 hours. The solvent was evaporated under reduced pressure to give an oil. The oil was partitioned between chloroform and dilute sodium carbonate solution and extracted further with chloroform (4×100 ml). The chloroform extracts were combined, dried over magnesium sulphate, filtered and evaporated to give an oil. The oil was purified by column chromatography using dichloromethane then chloroform as eluant. The solid obtained was recrystallized from diethyl ether/ dichloromethane to give the title compound, 0.6 g, m.p. 135-137°.

1. temperatureunder reflux for 20 hours
2. customThe solvent was evaporated under reduced pressure
3. customto give an oil
4. customThe oil was partitioned between chloroform and dilute sodium carbonate solution
5. extractionextracted further with chloroform (4×100 ml)
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. customevaporated
9. customto give an oil
10. customThe oil was purified by column chromatography
11. customThe solid obtained
12. customwas recrystallized from diethyl ether/ dichloromethane