反应详情

DIPEA (77.35 mg, 0.60 mmol) was added to a stirred solution of biphenyl-4-carboxylicacid (2-oxo-2-piperazin-1-yl-ethyl)-amide TFA salt (70 mg, 0.16 mmol) in DMF (2 mL). HOBT (19.8 mg, 0.14 mmol) and EDCI.HCl (63.74 mg, 0.33 mmol) were then added. After 2 minutes 4-fluorobenzoic acid (18.6 mg, 0.133 mmol) was added and the resulting mixture was stirred overnight. The reaction mixture was diluted with cold water and the product was precipitated and filtered to afford 28 mg (46.7% yield) of biphenyl-4-carboxylicacid {2-[4-(4-fluoro-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide. LC-MS purity: 94.8%, 1H NMR Values: (CDCl3) δ 7.9 (d, 2H), 7.7-7.6 (q, 4H), 7.5-7.4 (m, 5H), 7.3 (t, 1H), 7.2-7.1 (t, 2H), 4.4 (d, 2H), 4.0-3.5 (d, 8H).

1. customthe product was precipitated
2. filtrationfiltered