反应详情

DIPEA (0.130 mL, 0.76 mmol) was added to a stirred solution of [(thiophene-2-carbonyl)-amino]-acetic acid (40 mg, 0.22 mmol) in DMF (1 mL). HOBT (35 mg, 0.26 mmol) and EDCI.HCl (49 mg, 0.26 mmol) were added, followed by the addition of piperazine-1-yl-(2-trifluoromethyl-phenyl)-methanone hydrochloride (70 mg, 0.24 mmol) at room temperature. The reaction mixture was stirred at room temperature overnight. Water was then added, and the product was extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure to afford thiophene-2-carboxylic acid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazine-1-yl]-ethyl}-amide in 54% yield. LC-MS purity: 98% 1H NMR (CDCL3): δ 7.78-7.44 (m, 5H), 7.34 (t, 1H), 7.10 (d, 2H), 4.40-4.18 (m, 2H), 4.08-3.82 (m, 2H), 3.80-3.50 (m, 4H).

1. extractionthe product was extracted with EtOAc
2. washThe organic layer was washed with brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated under reduced pressure