反应详情

To a solution of (E)-N-((dimethylamino)methylene)-3,4-dimethoxy-5-nitrobenzamide (1.12 g, 4 mmol) ethanol (30 mL) was added 3-carbamimidoyl-2-(trifluoromethyl)pyridine 1-oxide (0.82 g, 4 mmol). The reaction mixture was heated to reflux for 5 hours. It was cooled to room temperature and the solvent was removed by evaporation. The residue was then dissolved in dichloromethane/isopropanol mixture (50 mL, 70:30) and the organic phase was washed with water, dried over anhydrous magnesium sulphate, filtered and evaporated. The crude product was recrystallized from ethanol to give 3-(4-(3,4-dimethoxy-5-nitrophenyl)-1,3,5-triazin-2-yl)-2-(trifluoromethyl)pyridine 1-oxide, 1.27 g (75%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 5 hours
3. customthe solvent was removed by evaporation
4. dissolutionThe residue was then dissolved in dichloromethane/isopropanol mixture (50 mL, 70:30)
5. washthe organic phase was washed with water
6. dry with materialdried over anhydrous magnesium sulphate
7. filtrationfiltered
8. customevaporated
9. customThe crude product was recrystallized from ethanol