反応 #70937

反応方程式

(E)-N-((dimethylamino)methylene)-3,4-dimethoxy-5-nitrobenzamide

2-(trifluoromethyl)nicotinimidamide

→

2-(3,4-dimethoxy-5-nitrophenyl)-4-(2-(trifluoromethyl)pyridin-3-yl)-1,3,5-triazine

反応条件

後処理

1. 1
   温度The reaction mixture was heated
2. 2
   温度to reflux for 5 hours
3. 3
   その他the solvent was removed by evaporation
4. 4
   workup.DISSOLUTIONThe residue was then dissolved in a dichloromethane/isopropanol mixture (50 mL, 70:30)
5. 5
   洗浄the organic phase was washed with water
6. 6
   乾燥dried over anhydrous magnesium sulphate
7. 7
   ろ過filtered
8. 8
   その他evaporated
9. 9
   その他The crude product was recrystallized from ethanol

実験手順

To a solution of (E)-N-((dimethylamino)methylene)-3,4-dimethoxy-5-nitrobenzamide (1.12 g, 4 mmol) ethanol (30 mL) was added 2-(trifluoromethyl)nicotinimidamide (0.756 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 a 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 2-(3,4-dimethoxy-5-nitrophenyl)-4-(2-(trifluoromethyl)pyridin-3-yl)-1,3,5-triazine, 1.221 g (75%).

出典