反应详情

A mixture of 3.10 g (8.40 mmol) 4-[(4-bromophenyl)amino]-6-nitro-quinoline-3-carbonitrile, 155 ml ethanol, and 9.47 g (42.0 mmol) SnCl2 dehydrate was heated to reflux under N2. After 4 hours, removed heat and added ice water. Made basic with sodium bicarbonate and stirred for 2 hours. With mixture still basic, extracted with chloroform, stirred organic layer with Darco and dried with sodium sulfate. Filtered, stripped solvent and dried in vacuo, giving 2.265 g of brown-yellow solid: mass spectrum (electrospray m/e): M+H=339.0, 341.0.

1. temperaturewas heated
2. temperatureto reflux under N2
3. customremoved
4. temperatureheat
5. additionadded ice water
6. extractionWith mixture still basic, extracted with chloroform
7. stirringstirred organic layer with Darco
8. dry with materialdried with sodium sulfate
9. filtrationFiltered
10. customdried in vacuo