反应详情

DIPEA (96 mg, 0.12 mL, 0.74 mmol) was added to a stirred solution of 4-pyrazin-2-yl-benzoic acid (50 mg, 0.24 mmol) in DMF (2 mL). HOBT (40 mg, 0.23 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 hydrochloride salt (105 mg, 0.29 mmol) was added and the resulting mixture was stirred at room temperature overnight. Cold water was then added and then extrated with ethyl acetate. The organic layer was washed with brine and dried over Na2SO4 and concentrated under reduced pressure to afford 78 mg (63.4%) of N-{2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-4-pyrazin-2-yl-benzamide. LCMS Purity: 96.69%. 1H NMR (DMSO-d6): δ 9.4-9.3 (d, 1H), 8.8-8.7 (m, 2H), 8.7-8.6 (d, 1H), 8.3-8.2 (d, 1H), 8.1-8.0 (d, 2H), 7.9-7.6 (m, 3H), 7.6-7.5 (bt, 1H), 4.3-4.1 (m, 2H), 3.8-3.54 (m, 4H), 3.54-3.4 (m, 2H), 3.2-3.04 (m, 2H).

1. washThe organic layer was washed with brine
2. dry with materialdried over Na2SO4
3. concentrationconcentrated under reduced pressure