반응 #710471

반응 방정식

potassium carbonate

2-bromo-5-bromomethylpyridine

2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide

→

N-[1-((6-bromopyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroacetamide

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   온도in sequence, and the resulting mixture was heated
3. 3
   온도refluxed for 6 hours
4. 4
   기타was returned to room temperature
5. 5
   여과to filter insoluble materials
6. 6
   농축the filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   기타to precipitate a solid
9. 9
   기타thus the solid was collected
10. 10
    세척washed with diethyl ether
11. 11
    기타dried under reduced pressure in a desiccator
12. 12
    기타to obtain the subject material
13. 13
    기타Amount obtained 81 mg (yield 82%)

실험 절차

70 mg (0.28 mmol) of the 2-bromo-5-bromomethylpyridine obtained by the aforementioned method was dissolved in 10 ml of anhydrous acetonitrile, 54 mg (0.28 mmol) of 2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide synthesized by the method described in (1) of Synthetic Example P1 and 46 mg (0.34 mmol) of potassium carbonate were added thereto in sequence, and the resulting mixture was heated and refluxed for 6 hours. After the reaction was completed, the reaction solution was returned to room temperature to filter insoluble materials, and the filtrate was concentrated under reduced pressure. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected, washed with diethyl ether, and then dried under reduced pressure in a desiccator to obtain the subject material. Amount obtained 81 mg (yield 82%).

출처