반응 #710476

반응 방정식

2-chloro-5-chloromethyl pyridine

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

potassium carbonate

→

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

용매

acetonitrile

반응 조건

후처리

1. 1
   기타synthesized by the aforementioned method
2. 2
   온도the resulting mixture was heated
3. 3
   온도refluxed for 1 hours
4. 4
   기타was returned to room temperature
5. 5
   농축concentrated under reduced pressure
6. 6
   workup.ADDITIONDiethyl ether was added
7. 7
   기타to precipitate a solid
8. 8
   기타thus the solid was collected
9. 9
   기타dried
10. 10
    기타to obtain the subject material
11. 11
    기타Amount obtained 49 mg (yield 45%)

실험 절차

53 mg (0.33 mmol) of 2-chloro-5-chloromethyl pyridine dissolved in 6 ml of anhydrous acetonitrile was added to 68 mg (0.33 mmol) of the 2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide synthesized by the aforementioned method, and subsequently, 50 mg (0.36 mmol) of potassium carbonate was added thereto and the resulting mixture was heated and refluxed for 1 hours. After the reaction was completed, the reaction solution was returned to room temperature and then concentrated under reduced pressure. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected and dried to obtain the subject material. Amount obtained 49 mg (yield 45%).

출처