反応 #710476

反応方程式

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

溶媒

acetonitrile

反応条件

後処理

1. 1
   その他synthesized by the aforementioned method
2. 2
   温度the resulting mixture was heated
3. 3
   温度refluxed for 1 hours
4. 4
   その他was returned to room temperature
5. 5
   濃縮concentrated under reduced pressure
6. 6
   workup.ADDITIONDiethyl ether was added
7. 7
   その他to precipitate a solid
8. 8
   その他thus the solid was collected
9. 9
   その他dried
10. 10
    その他to obtain the subject material
11. 11
    その他Amount obtained 49 mg (yield 45%)

実験手順

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%).

出典