반응 #710464

반응 방정식

water

triethylamine

2-aminopyridine

trifluoroacetic acid

→

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

수율 71.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred for 10 minutes
2. 2
   기타The mixture was transferred to a separatory funnel
3. 3
   기타liquid separation
4. 4
   세척the organic layer was washed twice with 150 ml of water and twice with 150 ml of a 1% HCl aqueous solution
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure

실험 절차

25 g (270 mmol) of 2-aminopyridine was dissolved in 200 ml of anhydrous dichloromethane, 41 ml (30 g, 300 mmol) of triethylamine was added thereto, and the mixture was cooled to 0° C. 38 ml (57 g, 270 mmol) of anhydrous trifluoroacetic acid was added dropwise thereto over 15 minutes, and the resulting mixture was stirred at room temperature for 2 hours. After the reaction was completed, the reaction solution was injected into about 100 ml of iced water, and the mixture was stirred for 10 minutes. The mixture was transferred to a separatory funnel to perform liquid separation, and the organic layer was washed twice with 150 ml of water and twice with 150 ml of a 1% HCl aqueous solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 36 g (yield 71%) of 2,2,2-trifluoro-N-(pyridin-2(1H)-ylidene)acetamide.

출처