反应详情

To a stirred suspension of N-phenyl- 4-cyano-2,6-dinitroaniline (16.4 g, 57.8 mmol) and SnCl2, 2H2O (130.5 g, 0.58 mol) in abs. ethanol (300 ml) was added formic acid (90 ml) dropwise at ambient temperature. The reaction is exothermic. The reaction was allowed to proceed at ambient conditions overnight. The resultant mixture was rendered alkaline by addition of saturated, aqueous sodium carbonate and was filtered through Celite. The filtrate was extracted with dichloromethane. The organic extract was dried over magnesium sulphate and evaporated under reduced pressure. The residue was triturated in cold ethyl acetate to leave the title product (8.65 g, 64%).

1. customto proceed at ambient conditions overnight
2. filtrationwas filtered through Celite
3. extractionThe filtrate was extracted with dichloromethane
4. extractionThe organic extract
5. dry with materialwas dried over magnesium sulphate
6. customevaporated under reduced pressure
7. customThe residue was triturated in cold ethyl acetate