반응 #1332619

반응 방정식

Water

4-chloro-2,3-difluoro-6-nitroaniline

1-ethylpiperazine

potassium carbonate

→

title compounds

수율 63.1%

4-Chloro-3-(4-ethylpiperazin-1-yl)-2-fluoro-6-nitroaniline

수율 63.1%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   추출followed by extraction with ethyl acetate
3. 3
   세척The ethyl acetate layer was washed with saturated brine
4. 4
   건조dried on anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off
6. 6
   기타The residue was separated
7. 7
   기타purified on silica gel column chromatography (chloroform/methanol=50/1)

실험 절차

To a solution of 768 mg of 4-chloro-2,3-difluoro-6-nitroaniline (which was prepared by the method described in WO 98/56761 or WO 98/35977) and 629 mg of 1-ethylpiperazine in 5 ml of dimethylsulfoxide, 1.00 g of potassium carbonate was added, followed by 2 hours' stirring at 50° C. Water was added to the reaction liquid, followed by extraction with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried on anhydrous magnesium sulfate, and the solvent was distilled off. The residue was separated and purified on silica gel column chromatography (chloroform/methanol=50/1) to provide 704 mg of the title compounds.

출처