反应详情

温度

100 °C

tert-Butyl 6-bromo-4-oxospiro[chroman-2,4′-piperidine]-1′-carboxylate (1 g) and 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (682 mg) were dissolved in dioxane in a nitrogen atmosphere, and aqueous 2M Na2CO3 (10 ml) solution (3.8 mL) and tetrakis(triphenylphosphine)palladium (144 mg) were added thereto, and degassed. The reaction liquid was stirred overnight at 100° C., cooled to room temperature, then water was added thereto, and filtered through Celite. The filtrate was extracted with chloroform, 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 (hexane/EtOAc) to obtain the intended compound as a pale yellow solid.

1. additionwere added
2. customdegassed
3. customThe reaction liquid
4. temperaturecooled to room temperature
5. filtrationfiltered through Celite
6. extractionThe filtrate was extracted with chloroform
7. dry with materialthe organic layer was dried with sodium sulfate
8. customSodium sulfate was removed through filtration
9. concentrationthe filtrate was concentrated under reduced pressure
10. customthe residue was purified through silica gel column chromatography (hexane/EtOAc)