Acetic Anhydride → HCID 68196369, compound

Participants

Reaction Steps

Benzyl [({5-(benzyloxy)-2-[(1-{4-[5-(1-hydroxyethyl)pyridin-2-yl]phenyl}piperidin-4-yl)methyl]-6-methylpyrimidin-4-yl}carbonyl)amino]acetate (0.24 g, 0.35 mmol) obtained in Example 12-(3) was dissolved in dichloromethane (30 mL), and acetic anhydride (0.050 mL, 0.52 mmol) and triethylamine (1.8 mL) were added, followed by stirring at room temperature for 12 hours. Acetic anhydride (1.8 mL) and pyridine (0.90 mL) were added to the reaction solution, followed by stirring for further 12 hours, and subsequently a saturated aqueous sodium hydrogencarbonate solution was added, followed by extraction with ethyl acetate. After the organic layer was concentrated under reduced pressure, the resulting residue was purified by chromatography on a silica gel column (Moritex Corporation, elution solvent: hexane/ethyl acetate), and a fraction corresponding to the Rf value=0.40 (hexane/ethyl acetate=1/1) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (0.12 g, 0.17 mmol) as a yellow oil (yield 48%).

Provenance & Evidence