反应详情

2-(4-Methylpiperazin-1-yl)ethyl 4-nitrophenyl carbonate (Intermediate 4; 680 mg, 2.2 mmol) was dissolved in DMF (20 mL). DIPEA (0.76 mL, 4.4 mmol) and 4-(4-methoxyphenyl)piperazine (422 mg, 2.2 mmol) were added and the reaction mixture was stirred at room temperature for 24 hours, and the reaction mixture was then concentrated in vacuo. The residue was purified by normal phase column chromatography (eluting with DCM, followed by a 500:8:1 mixture of DCM:EtOH:NH3, followed by a 50:8:1 mixture of DCM:EtOH:NH3). The residue was recrystallised from EtOAc to give 2-(4-methyl-piperazin-1-yl)ethyl 4-(4-methoxyphenyl)piperazine-1-carboxylate (137 mg, 17%) as a white solid.

1. concentrationthe reaction mixture was then concentrated in vacuo
2. customThe residue was purified by normal phase column chromatography (
3. washeluting with DCM
4. additionfollowed by a 500:8:1 mixture of DCM
5. additionEtOH:NH3, followed by a 50:8:1 mixture of DCM
6. customThe residue was recrystallised from EtOAc