1,2-Dichloroethane → HCID 69937008, compound

Participants

Reaction Steps

To a solution of 5-[(4-methyl-1-piperazinyl)carbonyl]-2-[(phenylmethyl)oxy]benzoic acid (may be prepared as described in Description 51; 166 mg, 0.47 mmol), 3-pyridinamine (44.1 mg, 0.47 mmol), and EDC (90 mg, 0.47 mmol) in N,N-dimethylformamide (DMF) (4 mL) stirred under nitrogen at room temperature was added neat HOBT (71.7 mg, 0.47 mmol) in one charge. The reaction mixture was stirred at room temperature for 6 h. The mixture was diluted with water (50 ml), extracted with ethyl acetate (3×50 ml). The organic phase was washed with saturated brine (25 ml), dried over sodium sulfate, and evaporated in vacuo to give the crude product. The crude product was purified by Prep-HPLC (Gilson GX-281; Durashell 10 μm, 21.5*250 nm n; A: 10 mmol/water, B: MeCN, O-7.2 min, 35%-35%; 7.2-7.5 min, 35%-95%; 7.5-11.5 min, 95%; RT: 7.0 min) to yield the title compound as a white solid. 30 mg.

Provenance & Evidence