Réaction #710474

Équation de réaction

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

Solvants

acetonitrile

acetonitrile

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONadded
2. 2
   Températurethe resulting mixture was heated
3. 3
   Températurerefluxed for 140 minutes
4. 4
   Autrewas returned to room temperature
5. 5
   Filtrationto filter off insoluble materials
6. 6
   Concentrationthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   Autreto precipitate a solid
9. 9
   Autrethus the solid was collected
10. 10
    Autredried well
11. 11
    Autreto obtain the subject material
12. 12
    AutreAmount obtained 63 mg (yield 37%)

Mode opératoire

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%).

Source