HRID1920077
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
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%).
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 5 hours
- customthe solvent was removed by evaporation
- dissolutionThe residue was then dissolved in dichloromethane/isopropanol mixture (50 mL, 70:30)
- washthe organic phase was washed with water
- dry with materialdried over anhydrous magnesium sulphate
- filtrationfiltered
- customevaporated
- customThe crude product was recrystallized from ethanol