反应详情

DIPEA (92 mg, 0.12 mL, 0.71 mmol) was added to a stirred solution of 5-(2-fluoro-phenyl)-1H-pyrazole-3-carboxylic acid (59 mg, 0.28 mmol) in DMF (2 mL). HOBT (40 mg, 0.29 mmol) and EDCI (57 mg, 0.29 mmol) were then added at room temperature. After 2 minutes, 2-amino-1-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone (100 mg, 0.28 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and filtered the solid precipitated to afford 131 mg (91.6% yield) of 5-(2-fluoro-phenyl)-1H-pyrazole-3-carboxylic acid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-amide. LCMS Purity: 95.28%. 1H NMR (DMSO-d6): δ 13.8 (d, 1H), 8.0 (m, 1H), 7.6 (m, 3H), 7.2 (m, 4H), 7.1 (m, 1H), 4.1 (d, 2H), 3.5 (m, 4H), 3.35 (m, 2H), 3.0 (m, 2H).

1. filtrationfiltered the solid
2. customprecipitated