反应详情

温度

10 °C

HOBt (21.5 mg, 0.16 mmol) and DIPEA (66 mg, 0.51 mmol) were added to a stirred solution of 5-phenyl-isoxazole-3-carboxylic acid (24 mg, 0.13 mmol) in DMF (1.0 mL). The mixture was then cooled to 10° C. and EDCI.HCl (30.5 mg, 0.16 mmol) followed by 2-amino-1-[4-(2-bromo-5-methoxy-benzoyl)-piperazin-1-yl]-ethanone hydrochloride (50 mg, 0.13 mmol) were added. The reaction mixture was then stirred at room temperature overnight. Water was added, and the resulting precipitate was isolated by filtration under reduced pressure and dried to afford 5-phenyl-isoxazole-3-carboxylic acid {2-[4-(2-bromo-5-methoxy-benzoyl)-piperazin-1-yl]-2-oxo-ethyl}-amide as a solid in 53.8% yield. LC-MS purity: 92.97%, 1H-NMR (DMSO): δ 8.7 (t, 1H), 8.0 (m, 2H), 7.58 (m, 4H), 7.41 (s, 1H), 7.0 (m, 2H), 4.2 (m, 2H), 3.78 (s, 3H), 3.5 (m, 6H), 3.2 (m, 2H).

1. additionwere added
2. customthe resulting precipitate was isolated by filtration under reduced pressure
3. customdried