反应详情

A mixture of 5-{4-[3-(2,6-dichloro-phenyl)-5-isopropyl-isoxazol-4-ylmethoxy]-2-methyl-phenyl}-thiophene-2-carboxylic acid (250 mg, 0.5 mmol), 1-[3-(dimethylamino) propyl]-3-ethylcarbodiimide hydrochloride (144 mg, 0.75 mmol), N,N′-dimethylamino pyridine (122 mg, 1.0 mmol) and methanesulfonamide (57 mg, 0.6 mmol) in dichloromethane (20 mL) is stirred at ambient temperature overnight. The reaction mixture is diluted with dichloromethane and washed with 1N HCl. The organic phase is concentrated under reduced pressure and purified by column chromatography (gradient: 0 to 20% EtOAc in hexanes with 0.1% AcOH) to give the title compound (160 mg, 55%). LC-ES/MS m/e 579 (M+1), 100%.

1. washwashed with 1N HCl
2. concentrationThe organic phase is concentrated under reduced pressure
3. custompurified by column chromatography (gradient: 0 to 20% EtOAc in hexanes with 0.1% AcOH)