반응 #710469

반응 방정식

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

용매

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   온도in sequence, and the resulting mixture was heated
3. 3
   온도refluxed for 6 hours
4. 4
   기타was returned to room temperature
5. 5
   여과to filter insoluble materials
6. 6
   농축the filtrate was concentrated under reduced pressure
7. 7
   기타The filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1)
8. 8
   기타to obtain the subject material
9. 9
   기타Amount obtained 21 mg (yield 23%)

실험 절차

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%).

출처