反应详情

温度

60 °C

To 14.00 g of N-[2-(3,5-dichloropyridin-2-yl)-2-nitroethyl]-2-(trifluoromethyl)benzamide in 70 ml of a mixture of N,N-dimethylformamide-water (7:1), 16.62 g of sodium nitrite was added, and the mixture was stirred at 60° C. for 18 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, poured into 100 ml of water and extracted with ethyl acetate (100 ml×2). The resulting organic layers were combined, washed with water (50 ml×1) and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 3:7 to 1:1) as the eluent to obtain 5.90 g of the desired product as pale yellow crystals.

1. customAfter completion of the reaction
2. temperatureto cool to room temperature
3. extractionextracted with ethyl acetate (100 ml×2)
4. washwashed with water (50 ml×1)
5. dry with materialdried over saturated aqueous sodium chloride
6. customanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography