反应详情

EDC (113 mg, 0.591 mmol) was added to a solution of 2-(4-nitrophenyl) propionic acid (92 mg, 0.473 mmol), Hunig's Base (0.083 ml, 0.473 mmol) and 1-[2-(4-Nitrophenyl)ethyl]piperazine hydrochloride (107 mg, 0.394 mmol) in 5 ml DCM and stirred at room temperature for 3 hours. The crude mixture was diluted with ethyl acetate and washed with saturated solution of NH4Cl, brine, dried over sodium sulfate, filtered and concentrated. Residue was purified by prep-TLC plate with 5% (NH4OH:MeOH 9:1) in DCM to yield 1-[2-(4-nitrophenyl)ethyl]-4-[2-(4-nitrophenyl)propanoyl]piperazine (100 mg, 0.24 mmol). 1H-NMR (500 MHz, DMSO) δ ppm 8.19 (d, J=9 Hz, 2H), 8.11 (d, J=9 Hz, 2H), 7.54 (d, J=9.Hz, 2H), 7.48 (d, J=9.Hz, 2H), 4.33 (q, 1H), 3.39-3.48 (m, 3H), 3.26-3.42 9 m, 2H), 2.82 (t, J=7.0 Hz, 2H), 2.5 (b, 1H), 2.35-2.40 (m, 2H), 2.26 (b, 1H), 2.0 (b, 1H), 1.30 (d, J=7 Hz, 3H).

1. washwashed with saturated solution of NH4Cl, brine
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customResidue was purified by prep-TLC plate with 5% (NH4OH:MeOH 9:1) in DCM