反应详情

温度

90 °C

Potassium carbonate (14.7 g, 106 mmol) and benzyl chloride (12.2 mL, 106 mmol) were added to a solution of 3-hydroxy-4-(3-methoxypropoxy)benzaldehyde described in Production Example 32-1 (17.2 g, 81.7 mmol) in ethanol (200 mL) under nitrogen atmosphere at room temperature, and the mixture was stirred under a thermal condition of 90° C. for 2 hours. The reaction liquid was cooled to 0° C., and the mixture was diluted with 2 M hydrochloric acid, ethyl acetate, and water. The organic layer was washed with a saturated saline solution and then dried over anhydrous magnesium sulfate. The drying agent was separated by filtration and then the filtrate was concentrated under vacuum. The residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=4:1-3:7) to obtain the title compound (19.8 g, 81%).

1. customThe reaction liquid
2. temperaturewas cooled to 0° C.
3. washThe organic layer was washed with a saturated saline solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe drying agent was separated by filtration
6. concentrationthe filtrate was concentrated under vacuum
7. customThe residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=4:1-3:7)