Reacción #710474

Ecuación de reacción

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

Disolventes

acetonitrile

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONadded
2. 2
   Temperaturathe resulting mixture was heated
3. 3
   Temperaturarefluxed for 140 minutes
4. 4
   Otrowas returned to room temperature
5. 5
   Filtraciónto filter off insoluble materials
6. 6
   Concentraciónthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONEther was added
8. 8
   Otroto precipitate a solid
9. 9
   Otrothus the solid was collected
10. 10
    Otrodried well
11. 11
    Otroto obtain the subject material
12. 12
    OtroAmount obtained 63 mg (yield 37%)

Procedimiento

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%).

Fuente