反应详情

To a stirred solution of (Z)-3-carbamohydrazonoyl-2-(trifluoromethyl)pyridine 1-oxide (1.10 g, 5 mmol) in ethanol (30 mL) was added 2-(3,4-dimethoxy-5-nitrophenyl)-2-oxoacetaldehyde (1.19 g, 5 mmol). The reaction mixture was heated to reflux for 5 hours, and then cooled to room temperature and the solvent was removed by evaporation. The residue was dissolved in dichloromethane (30 mL) and the organic phase was washed with water and dried over anhydrous magnesium sulphate, filtered and evaporated. The crude product was recrystallized from isopropanol to give 3-(5-(3,4-dimethoxy-5-nitrophenyl)-1,2,4-triazin-3-yl)-2-(trifluoromethyl)pyridine 1-oxide, 1.69 g (80%).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 5 hours
3. customthe solvent was removed by evaporation
4. dissolutionThe residue was dissolved in dichloromethane (30 mL)
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 isopropanol