反应详情

温度

90 °C

Methyl 4-bromo-3,5-diethoxybenzoate (1 g) and 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (895 mg) were dissolved in DME in a nitrogen atmosphere, and potassium phosphate (2.1 g) and 1,1′-bis(diphenylphosphino)ferrocene palladium (D) chloride-CH2Cl2 complex (269 mg) were added to it at room temperature, and degassed. The reaction liquid was stirred overnight at 90° C., then cooled to room temperature, and water was added to it, and this was filtered through Celite. The filtrate was extracted with chloroform, washed with saturated saline water, and 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 (hexane/ethyl acetate=100/0 to 50/50 to 35/65) to obtain the title compound as a pale yellow solid.

1. additionwere added to it at room temperature
2. customdegassed
3. customThe reaction liquid
4. temperaturecooled to room temperature
5. filtrationthis was filtered through Celite
6. extractionThe filtrate was extracted with chloroform
7. washwashed with saturated saline water
8. dry with materialdried 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 (hexane/ethyl acetate=100/0 to 50/50 to 35/65)