反应详情

温度

90 °C

Commercially available 1-(t-butoxycarbonyl)pyrrole-2-boronic acid (10.06 g, 47.7 mmol) was dissolved in a mixed solvent of 1,2-dimethoxyethane (150 mL) and water (25 mL), and 2-bromothiazole (4.40 mL, 48.8 mmol), palladium (II) acetate (535 mg, 2.38 mmol), triphenylphosphine (2.50 g, 9.53 mmol) and potassium carbonate (19.50 g, 141 mmol) were added, followed by stirring at 90° C. for 16 hours under nitrogen atmosphere. The reaction solution was cooled to room temperature, water (300 mL) and ethyl acetate (400 mL) were added, and the solution was separated. The organic layer was washed with saturated brine, and subsequently dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=0%-20%) to afford the desired compound (6.71 g, yield 56%) as a pale yellow oil.

1. additionwere added
2. temperatureThe reaction solution was cooled to room temperature
3. customthe solution was separated
4. washThe organic layer was washed with saturated brine
5. dry with materialsubsequently dried over sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe resulting residue was purified
8. washsilica gel column chromatography (elution solvent: ethyl acetate/hexane=0%-20%)