تفاعل #710474

معادلة التفاعل

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

المذيبات

acetonitrile

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONadded
2. 2
   درجة الحرارةthe resulting mixture was heated
3. 3
   درجة الحرارةrefluxed for 140 minutes
4. 4
   أخرىwas returned to room temperature
5. 5
   ترشيحto filter off insoluble materials
6. 6
   تركيزthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   أخرىto precipitate a solid
9. 9
   أخرىthus the solid was collected
10. 10
    أخرىdried well
11. 11
    أخرىto obtain the subject material
12. 12
    أخرىAmount obtained 63 mg (yield 37%)

الإجراء التجريبي

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%).

المصدر