反应详情

温度

120 °C

(±)-tert-Butyl 4-((1-(5-bromo-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-7-yl)ethoxy)methyl)-4-(4-fluorophenyl)piperidine-1-carboxylate (75 mg, 0. 113 mmol), tetrakis(triphenylphosphine) palladium(0) (13.1 mg, 0.011 mmol) and cyanozinc (20.7 mg, 0.226 mmol) were combined in dry N,N-dimethylformamide (2 mL) in a microwave tube and sealed. After flushing the mixture with nitrogen, the mixture was heated at 120° C. for 1 h via microwave. After cooling to room temperature, the reaction mixture was concentrated, dissolved in ethyl acetate and washed with water and brine, concentrated and purified by flash chromatography on silica gel (20% EtOAc/Hex) to afford 21 mg (30.5%) as an oil. LC/MS (HPLC method 2): tR=3.265 min, 609.18(MH)+.

1. customsealed
2. customAfter flushing the mixture with nitrogen
3. temperatureAfter cooling to room temperature
4. concentrationthe reaction mixture was concentrated
5. dissolutiondissolved in ethyl acetate
6. washwashed with water and brine
7. concentrationconcentrated
8. custompurified by flash chromatography on silica gel (20% EtOAc/Hex)
9. customto afford 21 mg (30.5%) as an oil