反应详情

1-(4-Chloro-3-nitro-benzenesulphonyl)-4-methyl-piperazine (0.50 g, 1.57 mmol) and benzylamine (0.502 g, 4.70 mmol) were dissolved in THF (10 ml) and heated at reflux for 3 h. The reaction mixture was then reduced in vacuo and partitioned between ethyl acetate and water. The organics were washed with brine, dried (MgSO4) and reduced in vacuo, and the resultant residue purified by column chromatography eluting with 0-10% methanol in ethyl acetate to give benzyl-[4-(4-methyl-piperazine-1-sulphonyl)-2-nitro-phenyl]-amine as a yellow solid (0.53 g, 86%). (LC/MS: Rt 2.21, [M+H]+ 391.05).

1. temperatureheated
2. temperatureat reflux for 3 h
3. custompartitioned between ethyl acetate and water
4. washThe organics were washed with brine
5. dry with materialdried (MgSO4)
6. customthe resultant residue purified by column chromatography
7. washeluting with 0-10% methanol in ethyl acetate