反応 #710474

反応方程式

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

溶媒

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONadded
2. 2
   温度the resulting mixture was heated
3. 3
   温度refluxed for 140 minutes
4. 4
   その他was returned to room temperature
5. 5
   ろ過to filter off insoluble materials
6. 6
   濃縮the filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   その他to precipitate a solid
9. 9
   その他thus the solid was collected
10. 10
    その他dried well
11. 11
    その他to obtain the subject material
12. 12
    その他Amount obtained 63 mg (yield 37%)

実験手順

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%).

出典