Réaction #710471

Équation de réaction

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

Solvants

acetonitrile

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONwere added
2. 2
   Températurein sequence, and the resulting mixture was heated
3. 3
   Températurerefluxed for 6 hours
4. 4
   Autrewas returned to room temperature
5. 5
   Filtrationto filter insoluble materials
6. 6
   Concentrationthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   Autreto precipitate a solid
9. 9
   Autrethus the solid was collected
10. 10
    Lavagewashed with diethyl ether
11. 11
    Autredried under reduced pressure in a desiccator
12. 12
    Autreto obtain the subject material
13. 13
    AutreAmount obtained 81 mg (yield 82%)

Mode opératoire

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%).

Source