Triethylamine → HCID 25167326, compound

Participants

Reaction Conditions

Reaction Steps

Et3N (42 mg, 0.42 mmol) was added to a stirred solution of 2-amino-1[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethanone (80 mg, 0.19 mmol) in DCM (4 mL) at 0-5° C. 4-biphenylsulfonyl chloride (47 mg, 0.19 mmol) was then added and the mixture was stirred at 0-5° C. for 4 hrs. The reaction was then diluted with cold water and the product was extracted with DCM, washed with 5% NaHCO3, 5% HCl, then saturated brine solution. The DCM layer was dried over sodium sulphate and concentrated. The residue was purified by column chromatography (using silica gel of 60-120 mesh and 60% EtOAc in hexane as eluent) to afford 33 mg (33.4% yield) of biphenyl-4-sulfonicacid {2-oxo-2-[4-(2-trifluoromethyl-benzoyl)-piperazin-1-yl]-ethyl}-amide. LC-MS purity: 90.35%. 1H-NMR (CDCl3) δ 7.9 (m, 2H), 7.7 (d, 3H,), 7.6-7.5 (m 4H), 7.5-7.4 (m, 3H), 7.3 (m, 1H), 5.6 (s, 1H), 4.0-3.7 (m, 5H), 3.7-3.5 (m, 3H), 3.4-3.3 (m, 2H), 3.25-3.1 (m, 3H).

Provenance & Evidence