反应详情

A solution of 5-bromo-1-isopropyl-6-methyl-4-oxo-1,4-dihydro-pyridine-3-carboxylic acid (preparation 3c, 0.50 g, 1.82 mmol), HBTU (0.77 g, 2.03 mmol), DIPEA (0.76 mL, 4.47 mmol) in DMF (2 mL) is stirred for 10 min. Then, 4-methylsulfonylbenzylamine hydrochloride (0.64 g, 2.89 mmol) is added and the reaction mixture is stirred for 72 h at room temperature. The reaction mixture is diluted with methanol, acidified with acetic acid and purified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.1% TFA, 60° C.). Yield: 0.25 g (31% of theory); ESI mass spectrum: [M+H]+=441 (bromine isotope pattern); Retention time HPLC: 1.16 min (Z002_006).

1. custompurified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.1% TFA, 60° C.)
2. custom1.16 min (Z002_006)