反应详情

A mixture of 6.0 g (16.8 mmol) of 6-nitro-4-(3-trifluoromethylphenylamino)quinoline-3-carbonitrile and 18.9 g (83.8 mmol) of SnCl2.2H2O in 240 mL of EtOH was refluxed under N2 for 1 hr. Ice water was added followed by NaHCO3 to pH 8. The mixture was stirred for 2 hr and then extracted with CHCl3. Darco was added and the extracts were filtered through anhyd MgSO4 and evaporated. The residue was filtered through silica gel with 10% MeOH in CHCl3. Solvent evaporation and drying in vacuo (40° C.) gave 4.87 g of 6-amino-4-(3-trifluoromethylphenylamino)quinoline-3-carbonitrile as a brown solid: mass spectrum (electrospray, m/e): M+H 329.1.

1. temperaturewas refluxed under N2 for 1 hr
2. extractionextracted with CHCl3
3. additionDarco was added
4. filtrationthe extracts were filtered through anhyd MgSO4
5. customevaporated
6. filtrationThe residue was filtered through silica gel with 10% MeOH in CHCl3
7. customSolvent evaporation
8. customdrying in vacuo (40° C.)