反应详情

To a mixture of 4-(4-fluoro-butyl)-pyridine-2-carboxylic acid methyl ester (0.24 g) in THF (3 mL) and water (1 mL) was added lithium hydroxide monohydrate (71.3 mg, 1.7 mmol, 1.5 equiv). The mixture was stirred at rt overnight and diluted with methanol (20 mL). Then H+ resin was added and the mixture was shaken for 10 minutes. The resin was washed with methanol (1×), 1:1 acetonitrile/water (1×), and acetonitrile (1×). The product was eluted with 5% TEA in methanol (4×) and acetonitrile (1×). The combined organic solvents were evaporated and co-evaporated with toluene to provide 4-(4-Fluoro-butyl)-pyridine-2-carboxylic acid (0.22 g, 65%).

1. additionThen H+ resin was added
2. stirringthe mixture was shaken for 10 minutes
3. washThe resin was washed with methanol (1×), 1:1 acetonitrile/water (1×), and acetonitrile (1×)
4. washThe product was eluted with 5% TEA in methanol (4×) and acetonitrile (1×)
5. customThe combined organic solvents were evaporated