반응 #2033438

반응 방정식

3-chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile

ethanol

NaOH

→

title compound

3-Chloro-5-(4-methyl-piperazin-1-yl)-benzoic acid

용매

HCl

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도was heated
3. 3
   온도at reflux for 20 hours
4. 4
   기타partitioned between EtOAc and H2O
5. 5
   기타The organic layer was evaporated to dryness in vacuo

실험 절차

To 3-chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile (1.4 g, 5.9 mmol) dissolved in ethanol (10 ml) was added 2M NaOH (20 ml) and reaction mixture was heated at reflux for 20 hours. The mixture was reduced in vacuo and the crude product was acidified in 1N HCl to pH 6 and partitioned between EtOAc and H2O. The organic layer was evaporated to dryness in vacuo to give 0.7 g of the title compound as a white solid (LC/MS: Rt 1.67, [M+H]+ 256, acidic method).

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