反应详情

温度

10 °C

HOBt (57 mg, 0.42 mmol) and DMAP (46 mg, 0.38 mmol) were added to a stirred solution of 3-oxo-3-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-propionic acid (60 mg, 0.35 mmol) in DMF (2 mL). The reaction mixture was cooled to 10° C. and EDCI.HCl (81 mg, 0.42 mmol) followed by 5-phenyl-pyridin-2-ylamine (120 mg, 0.35 mmol) were added. The reaction mixture was stirred at the room temperature overnight, then diluted with water and the product extracted with ethyl acetate. The ethyl acetate was washed with brine solution, dried over Na2SO4 and evaporated. The residue was purified by column chromatography using silica gel 60-120 mesh and 80% ethyl acetate in hexane as the eluant to afford 65 mg (38% 0 of 3-oxo-N-(5-phenyl-pyridin-2-yl)-3-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-propionamide. LCMS: 497.18 (M+1)+, 90.4%, 1H NMR: (CDCl3): δ 9.6 (d, 1H), 8.5 (s, 1H), 8.2 (m, 1H), 7.9 (m, 1H), 7.75 (d, 1H), 7.6 (m, 4H), 7.45 (t, 2H), 7.35 (m, 2H), 4.0 (m, 2H), 3.7 (m, 3H), 3.55 (m, 4H), 3.26 (m, 2H).

1. additionwere added
2. extractionthe product extracted with ethyl acetate
3. washThe ethyl acetate was washed with brine solution
4. dry with materialdried over Na2SO4
5. customevaporated
6. customThe residue was purified by column chromatography