反应详情

温度

25 °C

A slurry of 6.00 g (16.8 mmol) of 6-nitro-4-[(3-trifluoromethylphenyl)amino]quinoline-3-carbonitrile and 18.9 g (83.3 mmol) of SnCl2 dihydrate in 240 mL of ethanol was refluxed under N2 for 1 h. After cooling to 25° C., the reaction was diluted with ice water, neutralized with sodium bicarbonate and stirred for 2 h. The product was extracted with chloroform, treated with Darco, dried(magnesium sulfate) and evaporated. The residue was filtered through silica gel (10% methanol in chloroform), evaporated and dried in vacuo (40° C.) to give 4.87 g of brown solid: mass spectrum (electrospray, m/e): M+H 329.

1. extractionThe product was extracted with chloroform
2. additiontreated with Darco, dried(magnesium sulfate)
3. customevaporated
4. filtrationThe residue was filtered through silica gel (10% methanol in chloroform)
5. customevaporated
6. customdried in vacuo (40° C.)