反应详情

温度

10 °C

HOBt (34 mg, 0.25 mmol) and DIPEA (67.9 mg, 0.51 mmol) were added to a stirred solution of 2-chloro-5-trifluoromethylbenzoic acid (48 mg, 0.21 mmol) in DMF (3 mL). The reaction mixture was cooled to 10° C. and EDCI.HCl (48 mg, 0.25 mmol) followed by N-biphenyl-4-yl-3-oxo-3-piperazin-1-yl-propionamide hydrochloride (75 mg, 0.2 mmol) were added. The reaction mixture was stirred at room temperature overnight then diluted with water and 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 (60% ethyl acetate in hexane) to afford 53 mg (48%) of N-biphenyl-4-yl-3-[4-(2-chloro-5-trifluoromethyl-benzoyl)-piperazin-1-yl]-3-oxo-propionamide. LCMS: 530.14 (M+1)+ 98.5%, 1H NMR: (CDCl3): δ 9.6 (d, 1H), 7.6 (m, 8H), 7.43 (t, 2H), 7.33 (t, 1H), 4.0 (m, 2H), 3.7 (m, 4H), 3.5 (d, 2H), 3.3 (m, 2H).

1. additionwere added
2. extractionextracted 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