Reaktion #710474

Reaktionsgleichung

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

Lösungsmittel

acetonitrile

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONadded
2. 2
   Temperaturthe resulting mixture was heated
3. 3
   Temperaturrefluxed for 140 minutes
4. 4
   Sonstigewas returned to room temperature
5. 5
   Filtrationto filter off insoluble materials
6. 6
   Einengenthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   Sonstigeto precipitate a solid
9. 9
   Sonstigethus the solid was collected
10. 10
    Sonstigedried well
11. 11
    Sonstigeto obtain the subject material
12. 12
    SonstigeAmount obtained 63 mg (yield 37%)

Vorschrift

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%).

Quelle