반응 #1151547

반응 방정식

water

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

1-piperazine ethanol

potassium carbonate

→

title compound

수율 67.3%

4-Chloro-6-fluoro-2-nitro-5-[4-(2-hydroxyethyl)piperazin-1-yl]-aniline

수율 67.3%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   workup.WAITfollowed by an hour
2. 2
   온도After cooling
3. 3
   기타the reaction liquid to room temperature
4. 4
   추출followed by extraction with chloroform
5. 5
   건조The chloroform layer was dried on anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONthe solvent was distilled off

실험 절차

To a solution of 6.79 g of 4-chloro-2,3-difluoro-6-nitroaniline (which was synthesized following WO9856761 or WO9835977) and 4.70 g of 1-piperazine ethanol in 30 ml of dimethylsulfoxide, 9.23 g of potassium carbonate was added, followed by an hour's stirring at 50° C. After cooling the reaction liquid to room temperature, water was added thereto, followed by extraction with chloroform. The chloroform layer was dried on anhydrous magnesium sulfate, the solvent was distilled off and 6.98 g of the title compound in crude form was obtained as a yellow oily substance.

출처