反应 #710474

反应方程式

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

溶剂

acetonitrile

acetonitrile

反应条件

后处理

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

实验过程

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%).

来源