反应详情

温度

85 °C

Methyl 4-bromo-3,5-diethoxybenzoate (456 mg) and 4-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-isoxazole (438 mg) were dissolved in THF in a nitrogen atmosphere, and potassium phosphate (954 mg), palladium acetate (33 mg) and dicyclohexyl-(2′,6′-dimethoxy-biphenyl-2-yl)-phosphane (62 mg) were added to it, and degassed. The reaction liquid was stirred overnight at 85° C., then cooled to room temperature, water was added to it, and filtered through Celite. The filtrate was extracted with chloroform, washed with saturated saline water, and the organic layer was dried with sodium sulfate. Sodium sulfate was removed through filtration, the filtrate was concentrated under reduced pressure, and the residue was purified through silica gel column chromatography (hexanelethyl acetate=100/0 to 80/20) to obtain the title compound as a pale yellow solid.

1. additionwere added to it
2. customdegassed
3. customThe reaction liquid
4. temperaturecooled to room temperature
5. filtrationfiltered through Celite
6. extractionThe filtrate was extracted with chloroform
7. washwashed with saturated saline water
8. dry with materialthe organic layer was dried with sodium sulfate
9. customSodium sulfate was removed through filtration
10. concentrationthe filtrate was concentrated under reduced pressure
11. customthe residue was purified through silica gel column chromatography (hexanelethyl acetate=100/0 to 80/20)