反应详情

A stirred solution of 1-benzylpiperazine (8.81 g, 50.0 mmol), 4-fluoronitrobenzene (5.31 mL, 50.0 mmol), and K2CO3 (6.90 g, 50.0 mmol) in ethanol is heated at reflux temperature under nitrogen for 18 h, cooled, diluted with water, and extracted with CH2Cl2. The combined extracts are dried over MgSO4 and concentrated in vacuo to give a solid residue. The solid is triturated with 20:80 ethyl acetate:hexanes and filtered. The filtercake is air-dried to afford the title compound as orange crystals, 8.45 g (57% yield), mp 218-219° C., characterized by NMR and mass spectral analyses.

1. temperatureat reflux temperature under nitrogen for 18 h
2. temperaturecooled
3. extractionextracted with CH2Cl2
4. dry with materialThe combined extracts are dried over MgSO4
5. concentrationconcentrated in vacuo
6. customto give a solid residue
7. customThe solid is triturated with 20:80 ethyl acetate
8. filtrationhexanes and filtered
9. customThe filtercake is air-dried