반응 #1010977

반응 방정식

3-bromo-5-trifluoromethyl-pyridin-2-yl-amine

acetylacetone

cesium carbonate

ammonia

NMP

ammonium chloride

→

N2-methyl-5-trifluoromethylpyridin-2,3-diamin

반응 조건

후처리

1. 1
   workup.WAITat 130° C. for 3 hours
2. 2
   온도to cool to room temperature
3. 3
   추출extracted with ethyl acetate
4. 4
   건조The organic layer was dried over sodium sulfate
5. 5
   농축concentrated under reduced pressure

실험 절차

To a pressure-resistant reaction container, N-methyl-(3-bromo-5-trifluoromethyl-pyridin-2-yl-amine (0.51 g), copper (II) acetylacetone (0.11 g), acetylacetone (0.20 g), cesium carbonate (1.30 g), NMP (2 ml), and 28% of aqueous ammonia (1 ml) were added, and stirred at 120° C. for 7 hours, then at 130° C. for 3 hours. The mixture was allowed to cool to room temperature, and then saturated aqueous ammonium chloride solution was poured, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 0.28 g of N2-methyl-5-trifluoromethylpyridin-2,3-diamin.

출처