반응 #427663

반응 방정식

3-bromo-2-chloro-5-nitropyridine

Potassium carbonate

phenol

N,N-dimethylacetamide

→

3-nitrobenzofuro[2,3-b]pyridine

수율 52.2%

용매

Water

반응 조건

후처리

1. 1
   workup.STIRRINGby stirring at 100° C. for 3.5 hours
2. 2
   추출followed by extraction with ethyl acetate
3. 3
   세척The resultant was washed with saturated saline
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONSubsequently, the solvent was distilled away under reduced pressure, hexane and ethyl acetate
6. 6
   workup.ADDITIONwere added to the obtained residue
7. 7
   여과an insoluble precipitate was collected by filtration

실험 절차

Potassium carbonate (87 mg) and phenol (47 mg) were added to an N,N-dimethylacetamide (1 ml) solution containing 3-bromo-2-chloro-5-nitropyridine (100 mg), followed by stirring at 70° C. for 3 hours. Acetic acid palladium (20 mg) was added in a nitrogen atmosphere, followed by stirring at 100° C. for 3.5 hours. Water was added, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, hexane and ethyl acetate were added to the obtained residue, an insoluble precipitate was collected by filtration, and a light yellow solid of 3-nitrobenzofuro[2,3-b]pyridine (47.1 mg) was thus obtained.

출처