反应详情

温度

80 °C

A mixture of 1-bromo-4-nitrobenzene (5 g, 24.8 mmol) and 1-benzylpiperazine (8.6 ml, 49.5 mmol, 2 equiv) is heated to 80° C. for 17 h. The reaction mixture is allowed to cool to RT, and is diluted with DCM/H2O. The layers are separated and the aqueous phase is extracted with DCM. The combined organic phase is washed with brine, dried (Na2SO4), filtered and concentrated. Purification of the residue by silica gel column chromatography (Hex/EtOAc, 1:1) affords the title compound as a yellow solid: ESI-MS: 298.3 [MH]+; tR=3.25 min (purity: 100%, system 1).

1. temperatureto cool to RT
2. customThe layers are separated
3. extractionthe aqueous phase is extracted with DCM
4. washThe combined organic phase is washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification of the residue by silica gel column chromatography (Hex/EtOAc, 1:1)