تفاعل #710471

معادلة التفاعل

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added
2. 2
   درجة الحرارةin sequence, and the resulting mixture was heated
3. 3
   درجة الحرارةrefluxed for 6 hours
4. 4
   أخرىwas returned to room temperature
5. 5
   ترشيحto filter insoluble materials
6. 6
   تركيزthe filtrate was concentrated under reduced pressure
7. 7
   workup.ADDITIONDiethyl ether was added
8. 8
   أخرىto precipitate a solid
9. 9
   أخرىthus the solid was collected
10. 10
    غسيلwashed with diethyl ether
11. 11
    أخرىdried under reduced pressure in a desiccator
12. 12
    أخرىto obtain the subject material
13. 13
    أخرىAmount obtained 81 mg (yield 82%)

الإجراء التجريبي

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%).

المصدر