反应详情

Lithium aluminum hydride (6.0 g, 0.16 mmol) is suspended in THF (500 ml), and thereto is added with stirring 3-(3-methoxymethoxypyridin-4-yl)propionic acid ethyl ester (21 g, 89 mmol) obtained in Reference Example 25 at 50° C. over a period of time for 30 minutes. The mixture is heated under reflux for 30 minutes, and thereto are added successively water (6 ml), a 15% sodium hydroxide (6 ml) and water (18 ml) in order to quench the reaction. The reaction solution is filtered to remove the insoluble materials, and the filtrate is concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: ethyl acetate) to give the title compound (17.5 g) as a colorless oil.

1. customobtained in Reference Example 25 at 50° C. over a period of time for 30 minutes
2. temperatureThe mixture is heated
3. temperatureunder reflux for 30 minutes
4. customa 15% sodium hydroxide (6 ml) and water (18 ml) in order to quench
5. customthe reaction
6. filtrationThe reaction solution is filtered
7. customto remove the insoluble materials
8. concentrationthe filtrate is concentrated under reduced pressure
9. customThe residue is purified by silica gel column chromatography (eluent: ethyl acetate)