反应详情

To a solution of 1-(4-cyano-benzyl)-6-methyl-4-oxo-1,4-dihydro-pyridine-3-carboxylic acid (preparation 1b, 12.9 g, 48.2 mmol) in glacial acetic acid (50 ml) is added at room temperature bromine (5.0 mL). The reaction mixture is stirred for 1 day at room temperature, then additional bromine (3.0 mL) is added. After stirring for an additional 4 days at room temperature, water is added to the reaction mixture and the formed precipitate is filtered off and dried. Yield: 14.0 g (84% of theory); ESI mass spectrum: [M+H]+=347 (bromine isotope pattern); Retention time HPLC: 1.07 min (Z002—005).

1. stirringAfter stirring for an additional 4 days at room temperature
2. filtrationthe formed precipitate is filtered off
3. customdried
4. custom1.07 min (Z002—005)