反应详情

温度

100 °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), sodium tert-butoxide (16.3 mg, 0.17 mmol), and palladium(II)acetate (1.02 mg, 4.53 μmol) were combined in toluene (2 mL) and treated with 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane (3.1 mg, 9.05 μmol) and morpholine (0.012 mL, 0.136 mmol) in a microwave tube and sealed. After flushing the mixture with nitrogen, the mixture was heated at 100° C. for 1 h via microwave. After cooling to room temperature, the reaction mixture was concentrated, dissolved in ethyl acetate, washed with water and brine, concentrated, and purified by flash chromatography on silica gel (30% EtOAc/Hex) to afford 44 mg (58%) as an oil. LC/MS (HPLC method 2): tR=3.185 min, 669.25(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 (30% EtOAc/Hex)
9. customto afford 44 mg (58%) as an oil