반응 #1010969

반응 방정식

ammonia

3-bromo-5-trifluoromethyl-pyridine-2-ylamine

acetylacetone

cesium carbonate

→

5-trifluoromethyl-pyridine-2,3-diamine

용매

NMP

water

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타After the reactor was sealed
3. 3
   온도with heating for 12 hours
4. 4
   온도cooled to room temperature
5. 5
   추출extracted with ethyl acetate
6. 6
   건조The combined organic layer was dried over sodium sulfate
7. 7
   농축concentrated under reduced pressure

실험 절차

To an autoclave reactor, 3-bromo-5-trifluoromethyl-pyridine-2-ylamine (40 g), acetylacetone copper(II) (2.2 g), acetylacetone (6.6 g), cesium carbonate (59 g), and NMP (105 ml) were added, and then 28% of aqueous ammonia solution (25 mL) was added under ice-cooling. After the reactor was sealed, the mixture heated to 110° C., and stirred with heating for 12 hours. The mixture was ice-cooled to room temperature, then diluted with water, and extracted with ethyl acetate. The combined organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 15 g 5-trifluoromethyl-pyridine-2,3-diamine (Compound (1F)-22).

출처