反応 #710471

反応方程式

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
   workup.ADDITIONDiethyl ether was added
8. 8
   その他to precipitate a solid
9. 9
   その他thus the solid was collected
10. 10
    洗浄washed with diethyl ether
11. 11
    その他dried under reduced pressure in a desiccator
12. 12
    その他to obtain the subject material
13. 13
    その他Amount obtained 81 mg (yield 82%)

実験手順

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%).

出典