反应详情

A mixture of 5.360 g (15.6 mmol) 4-[(3-chloro-4-fluorophenyl)amino]-6-nitro-quinoline-3-carbonitrile, 250 ml ethanol, and 17.67 g (78.2 mmol) SnCl2 dihydrate was heated to reflux under N2. Removed heat at 1½ hours and added ice water. Made basic with sodium bicarbonate. Stirred for 2 hours extracted with chloroform. Added brine to the separatory funnel to help separate layers. Stirred organic layer with Darco and dried with sodium sulfate. Filtered, stripped solvent and dried in vacuo, giving 4.460 g of yellow-brown solid: mass spectrum (electrospray m/e): M+H=312.9, 315.0.

1. temperaturewas heated
2. temperatureto reflux under N2
3. customRemoved
4. temperatureheat at 1½ hours
5. additionadded ice water
6. extractionextracted with chloroform
7. customAdded brine to the separatory funnel to help separate layers
8. dry with materialStirred organic layer with Darco and dried with sodium sulfate
9. filtrationFiltered
10. customdried in vacuo