반응 #1018179

반응 방정식

3-bromo-5-(trifluoromethyl)pyridin-2-amine

potassium 2-chloro-3-ethoxy-3-oxoprop-1-en-1-olate

sulfuric acid

ethanol

→

title compound

수율 62.0%

ethyl 8-bromo-6-(trifluoromethyl)imidazo[1,2-a]pyridine-3-carboxylate

수율 62.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with water
2. 2
   추출extracted with ethyl acetate
3. 3
   세척washed with water and saturated brine
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타the solvent was evaporated under reduced pressure
6. 6
   여과the obtained solid was collected by filtration

실험 절차

A mixture of 3-bromo-5-(trifluoromethyl)pyridin-2-amine (3.0 g), potassium 2-chloro-3-ethoxy-3-oxoprop-1-en-1-olate (5.4 g), sulfuric acid (0.80 mL) and ethanol (60 mL) was stirred overnight at 90° C. The reaction mixture was diluted with ethyl acetate, and washed with water. The aqueous layer was neutralized with 1N sodium hydroxide, and extracted with ethyl acetate. The organic layers were combined, washed with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was suspended in a mixed solvent of IPE and hexane, and the obtained solid was collected by filtration to give the title compound (2.6 g).

출처