反应详情

A solution of (1R)-1-{5-[3,5-dichloro-2-(methoxycarbonyl)phenyl]-3-fluoro-pyridin-2-yl}ethanaminium chloride (0.277 g, 0.73 mmol), 1-[(trifluoroacetyl)amino]cyclo-propanecarboxylic acid (0.160 g, 0.812 mmol), 1-ethyl-(3-dimethylaminopropyl)-carbodiimide hydrochloride (0.311 g, 1.62 mmol), 1-hydroxy-7-azabenzotriazole (0.010 g, 0.15 mmol), and triethylamine (0.45 mL, 3.25 mmol) in 5 mL CH2Cl2 was stirred at room temperature for 3 days. The solution was washed with aqueous sodium bicarbonate and brine, dried over Na2SO4, filtered and concentrated. The residue was subjected to silica gel chromatography eluted with 10–30% ethyl acetate in hexanes to provide methyl 2,4dichloro-6-(5-fluoro-6-{(1R)-1-[({1-[(trifluoroacetyl)amino]cyclopropyl}carbonyl)amino]ethyl}pyridin-3-yl)benzoate that gave proton NMR spectra consistent with theory and a mass ion (ES+) of 522.05 for M+H+.

1. washThe solution was washed with aqueous sodium bicarbonate and brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. washeluted with 10–30% ethyl acetate in hexanes