Réaction #710469

Équation de réaction

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

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
   AutreThe filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1)
8. 8
   Autreto obtain the subject material
9. 9
   AutreAmount obtained 21 mg (yield 23%)

Mode opératoire

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%).

Source