반응 #60124

반응 방정식

2,6-dichloro-3-nitropyridine

2,4-dichlorobenzeneboronic acid

Na2CO3

→

2-(2,4-dichlorophenyl)-6-chloro-3-nitropyridine

용매

THF

반응 조건

후처리

1. 1
   기타0.5 ml water and purged with nitrogen
2. 2
   농축The reaction mixture was concentrated in vacuo
3. 3
   workup.ADDITIONdiluted with water and ethyl acetate
4. 4
   추출The solution was extracted three times with ethyl acetate
5. 5
   건조dried over sodium sulfate
6. 6
   기타purified by column chromatography
7. 7
   세척eluting with 10% ethylacetate 90% hexanes

실험 절차

1 mmol 2,6-dichloro-3-nitropyridine, 1.05 mmol of 2,4-dichlorobenzeneboronic acid, and 3 mmol of Na2CO3, were dissolved in 1.5 ml THF and 0.5 ml water and purged with nitrogen. 0.05 mmol of [1,1′-Bis(diphenylphosphino)-ferrocene]dichloro-palladium(II) was added to reaction and stirred at room temperature under nitrogen for fourteen hours. The reaction mixture was concentrated in vacuo and diluted with water and ethyl acetate. The solution was extracted three times with ethyl acetate, dried over sodium sulfate, and purified by column chromatography eluting with 10% ethylacetate 90% hexanes to obtain 2-(2,4-dichlorophenyl)-6-chloro-3-nitropyridine.

출처