反应 #710471

反应方程式

potassium carbonate

2-bromo-5-bromomethylpyridine

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

→

N-[1-((6-bromopyridin-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
   workup.ADDITIONDiethyl ether was added
8. 8
   其他to precipitate a solid
9. 9
   其他thus the solid was collected
10. 10
    洗涤washed with diethyl ether
11. 11
    其他dried under reduced pressure in a desiccator
12. 12
    其他to obtain the subject material
13. 13
    其他Amount obtained 81 mg (yield 82%)

实验过程

70 mg (0.28 mmol) of the 2-bromo-5-bromomethylpyridine obtained by the aforementioned method was dissolved in 10 ml of anhydrous acetonitrile, 54 mg (0.28 mmol) of 2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetoamide synthesized by the method described in (1) of Synthetic Example P1 and 46 mg (0.34 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. Diethyl ether was added thereto to precipitate a solid, and thus the solid was collected, washed with diethyl ether, and then dried under reduced pressure in a desiccator to obtain the subject material. Amount obtained 81 mg (yield 82%).

来源