反应详情

DIPEA (350 mg, 0.5 mL, 2.7 mmol) was added to a stirred solution of 4-(4-methyl-piperazin-1-yl)-benzoic acid hydrochloride salt (116 mg, 0.45 mmol) in DMF (5 mL). HOBT (67 mg, 0.5 mmol) and EDCI (216 mg, 1.12 mmol) were then added at room temperature. After 2 minutes, 2-amino-1-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone hydrochloride salt (184 mg, 0.5 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and filtered the solid residue. The obtained residue was purified by preparative HPLC to afford 100 mg (41.3% yield) N-{2-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-4-(4-methyl-piperazin-1-yl)-benzamide. LCMS Purity: 88.3%. 1H NMR (DMSO-d6): δ 10.4 (s, 1H), 8.4 (s, 1H), 8.0 (t, 1H), 7.86 (d, 2H), 7.64 (m, 2H), 7.1 (d, 2H), 4.2-3.96 (m, 4H), 3.66-3.4 (m, 8H), 3.24-3.0 (m, 6H), 2.9 (s, 3H).

1. filtrationfiltered the solid residue
2. customThe obtained residue was purified by preparative HPLC