反応 #710469

反応方程式

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

溶媒

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   温度in sequence, and the resulting mixture was heated
3. 3
   温度refluxed for 6 hours
4. 4
   その他was returned to room temperature
5. 5
   ろ過to filter insoluble materials
6. 6
   濃縮the filtrate was concentrated under reduced pressure
7. 7
   その他The filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1)
8. 8
   その他to obtain the subject material
9. 9
   その他Amount obtained 21 mg (yield 23%)

実験手順

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%).

出典