反应详情

To a solution of 4-(pyridin-3-yloxy)benzoic acid (11.2 g, 52.0 mmol) in tetrahydrofuran (160 ml) was added N,N′-carbonyldiimidazole (9.28 g, 57.3 mmol), and the mixture was heated under reflux for 3 hrs. After cooling the reaction solution to room temperature, monobenzyl malonate magnesium salt (11.7 g, 28.6 mmol) was added, and the mixture was heated under reflux for 2 hrs. The reaction solution was concentrated and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to give the objective substance (14.1 g, 78%).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 3 hrs
3. temperaturethe mixture was heated
4. temperatureunder reflux for 2 hrs
5. concentrationThe reaction solution was concentrated
6. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1)
7. customto give the objective substance (14.1 g, 78%)