反应详情

A mixture of 5.734 g (13.1 mmol) 4-[3-chloro-4-(1-methyl-1H-imidazol-2-ylsulfanyl)-phenylamino]-6-nitro-quinoline-3-carbonitrile, 250 ml ethanol, and 14.83 g (65.6 mmol) tin chloride dihydrate was heated to reflux under N2. Removed heat at 2½ hours and added a large volume of ice water. Made basic with sodium bicarbonate and stirred for 2 hours. With mixture still basic, extracted with chloroform, stirred organic layer with Darco, dried with sodium sulfate and filtered. Stripped solvent and dried in vacuo, giving 2.86 g of yellow-brown solid: mass spectrum (electrospray m/e): M+H=407.3, 409.3.

1. temperaturewas heated
2. temperatureto reflux under N2
3. customRemoved
4. temperatureheat at 2½ hours
5. additionadded a large volume of 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. customStripped solvent and dried in vacuo