反应详情

温度

90 °C

Potassium carbonate (3.87 g, 28.0 mmol) and benzyl chloride (3.2 mL, 27.8 mmol) were added to a suspension of 4-(3-fluoropropoxy)-3-hydroxybenzaldehyde described in Production Example 33-1 (4.62 g, 23.3 mmol) in ethanol (46 mL) under nitrogen atmosphere at mom temperature, and the mixture was stirred at 90° C. for 1.5 hours. The reaction mixture was cooled to 0° C., then 2 M hydrochloric acid, ethyl acetate, and water were added for partition. The organic layer was washed with a saturated saline solution, dried over anhydrous magnesium sulfate, and then filtered. The solvent was evaporated and the resultant residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=9:1-3:2-1:1). The target fraction was concentrated under vacuum to obtain the title compound (6.14 g, 91%).

1. temperatureThe reaction mixture was cooled to 0° C.
2. customfor partition
3. washThe organic layer was washed with a saturated saline solution
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customThe solvent was evaporated
7. customthe resultant residue was purified with silica gel column chromatography (n-heptane:ethyl acetate=9:1-3:2-1:1)
8. concentrationThe target fraction was concentrated under vacuum