Реакция #710471

Уравнение реакции

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

Растворители

acetonitrile

Условия реакции

Обработка

1. 1
   workup.ADDITIONwere added
2. 2
   Температураin sequence, and the resulting mixture was heated
3. 3
   Температураrefluxed for 6 hours
4. 4
   Другоеwas returned to room temperature
5. 5
   Фильтрацияto filter insoluble materials
6. 6
   Концентрированиеthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   Другоеto precipitate a solid
9. 9
   Другоеthus the solid was collected
10. 10
    Промывкаwashed with diethyl ether
11. 11
    Другоеdried under reduced pressure in a desiccator
12. 12
    Другоеto obtain the subject material
13. 13
    ДругоеAmount obtained 81 mg (yield 82%)

Методика

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%).

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