反应 #710469

反应方程式

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

溶剂

acetonitrile

反应条件

后处理

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
   其他was returned to room temperature
5. 5
   过滤to filter insoluble materials
6. 6
   浓缩the filtrate was concentrated under reduced pressure
7. 7
   其他The filtrate was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→3:1)
8. 8
   其他to obtain the subject material
9. 9
   其他Amount obtained 21 mg (yield 23%)

实验过程

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%).

来源