反应详情

A mixture of 4.53 g (13.9 mmol) 4-[(3,4-difluorophenyl)amino]-6-nitro-3-quinolinecarbonitrile, 200 ml ethanol and 15.72 g (69.4 mmol) SnCl2 dihydrate was heated to reflux under N2. Removed heat at 1.5 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 1.5 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