反応 #427663

反応方程式

3-bromo-2-chloro-5-nitropyridine

Potassium carbonate

phenol

N,N-dimethylacetamide

→

3-nitrobenzofuro[2,3-b]pyridine

収率 52.2%

溶媒

Water

反応条件

後処理

1. 1
   workup.STIRRINGby stirring at 100° C. for 3.5 hours
2. 2
   抽出followed by extraction with ethyl acetate
3. 3
   洗浄The resultant was washed with saturated saline
4. 4
   乾燥dried 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
   ろ過an insoluble precipitate was collected by filtration

実験手順

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.

出典