Reacción #710471

Ecuación de reacción

potassium carbonate

2-bromo-5-bromomethylpyridine

2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide

→

N-[1-((6-bromopyridin-3-yl)methyl)pyridin-2(1H)-ylidene]-2,2,2-trifluoroacetamide

Disolventes

acetonitrile

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONwere added
2. 2
   Temperaturain sequence, and the resulting mixture was heated
3. 3
   Temperaturarefluxed for 6 hours
4. 4
   Otrowas returned to room temperature
5. 5
   Filtraciónto filter insoluble materials
6. 6
   Concentraciónthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   Otroto precipitate a solid
9. 9
   Otrothus the solid was collected
10. 10
    Lavadowashed with diethyl ether
11. 11
    Otrodried under reduced pressure in a desiccator
12. 12
    Otroto obtain the subject material
13. 13
    OtroAmount obtained 81 mg (yield 82%)

Procedimiento

70 mg (0.28 mmol) of the 2-bromo-5-bromomethylpyridine obtained by the aforementioned method was dissolved in 10 ml of anhydrous acetonitrile, 54 mg (0.28 mmol) of 2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide synthesized by the method described in (1) of Synthetic Example P1 and 46 mg (0.34 mmol) of potassium carbonate were added thereto in sequence, and the resulting mixture was heated and refluxed for 6 hours. After the reaction was completed, the reaction solution was returned to room temperature to filter insoluble materials, and the filtrate was concentrated under reduced pressure. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected, washed with diethyl ether, and then dried under reduced pressure in a desiccator to obtain the subject material. Amount obtained 81 mg (yield 82%).

Fuente