反应详情

A mixture of 4.53 g (13.9 mmol) 4-[(3,4-difluorophenyl)amino]-6-nitro-quinoline-3-carbonitrile, 200 ml ethanol and 15.72 g (69.4 mmol) SnCl2 dihydrate was heated to reflux under N2. Removed heat at 1½ hours, added ice water and made basic with sodium bicarbonate. Stirred for 2 hours and extracted with chloroform. Stirred organic layer with Darco, dried with sodium sulfate and filtered. Stripped solvent and dried in vacuo, giving 3.660 g of yellow-green solid: mass spectrum (electrospray m/e): M+H=297.1.

1. temperaturewas heated
2. temperatureto reflux under N2
3. customRemoved
4. temperatureheat at 1½ hours
5. additionadded ice water
6. extractionextracted with chloroform
7. dry with materialStirred organic layer with Darco, dried with sodium sulfate
8. filtrationfiltered
9. customStripped solvent and dried in vacuo