反应详情

DIPEA (124 mg, 0.16 mL, 0.95 mmol) was added to a stirred solution of 5-(2-trifluoromethyl-phenyl)-1H-pyrazole-3-carboxylic acid (70 mg, 0.27 mmol) in DMF (2 mL). HOBT (43 mg, 0.31 mmol) and EDCI (60 mg, 0.31 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 (101 mg, 0.27 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added, filtered the solid precipitate. The solid was purified by dissolving in DCM and washed with 1.2N HCl. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to afford 57 mg (36.77% yield) of 5-(2-trifluoromethyl-phenyl)-1H-pyrazole-3-carboxylic acid {2-[4-(5-fluoro-2-trifluoromethyl-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide. LCMS Purity: 93.30%. 1H NMR (DMSO-d6): δ 13.6 (s, 1H), 8.1 (m, 1H), 7.9 (m, 2H), 7.5 (m, 21H), 7.5 (m, 6H), 6.79 (s, 1H), 4.1 (d, 2H), 3.5 (m, 7H), 3.0 (m, 3H).

1. filtrationfiltered the solid precipitate
2. customThe solid was purified
3. dissolutionby dissolving in DCM
4. washwashed with 1.2N HCl
5. dry with materialThe organic phase was dried over Na2SO4
6. concentrationconcentrated under reduced pressure