Reaktion #710471

Reaktionsgleichung

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

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added
2. 2
   Temperaturin sequence, and the resulting mixture was heated
3. 3
   Temperaturrefluxed for 6 hours
4. 4
   Sonstigewas returned to room temperature
5. 5
   Filtrationto filter insoluble materials
6. 6
   Einengenthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   Sonstigeto precipitate a solid
9. 9
   Sonstigethus the solid was collected
10. 10
    Waschenwashed with diethyl ether
11. 11
    Sonstigedried under reduced pressure in a desiccator
12. 12
    Sonstigeto obtain the subject material
13. 13
    SonstigeAmount obtained 81 mg (yield 82%)

Vorschrift

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%).

Quelle