반응 #710474

반응 방정식

2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide

2-chloro-5-chloromethyl pyridine

potassium carbonate

→

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

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONadded
2. 2
   온도the resulting mixture was heated
3. 3
   온도refluxed for 140 minutes
4. 4
   기타was returned to room temperature
5. 5
   여과to filter off insoluble materials
6. 6
   농축the filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   기타to precipitate a solid
9. 9
   기타thus the solid was collected
10. 10
    기타dried well
11. 11
    기타to obtain the subject material
12. 12
    기타Amount obtained 63 mg (yield 37%)

실험 절차

100 mg (0.58 mmol) of the 2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide obtained by the aforementioned method was dissolved in 10 ml of anhydrous acetonitrile, 94 mg (0.58 mmol) of 2-chloro-5-chloromethyl pyridine was dissolved in 5 ml of anhydrous acetonitrile and added thereto, and subsequently, 84 mg (0.63 mmol) of potassium carbonate was added thereto and the resulting mixture was heated and refluxed for 140 minutes. After the reaction was completed, the reaction solution was returned to room temperature to filter off insoluble materials, and the filtrate was concentrated under reduced pressure. Ether was added thereto to precipitate a solid, and thus the solid was collected and dried well to obtain the subject material. Amount obtained 63 mg (yield 37%).

출처