Реакция #710469

Уравнение реакции

potassium carbonate

5-bromomethyl-2-fluoropyridine

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

→

N-[1-((6-fluoropyridin-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
   ДругоеThe filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1)
8. 8
   Другоеto obtain the subject material
9. 9
   ДругоеAmount obtained 21 mg (yield 23%)

Методика

57 mg (0.30 mmol) of the 5-bromomethyl-2-fluoropyridine obtained by the aforementioned method was dissolved in 10 ml of anhydrous acetonitrile, 57 mg (0.30 mmol) of 2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide synthesized by the method described in (1) of Synthetic Example P1 and 69 mg (0.50 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. The filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1) to obtain the subject material. Amount obtained 21 mg (yield 23%).

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