反应详情

温度

140 °C

In a 10 mL microwave vial were mixed (1R,5S)-3-(5-bromo-4-methylpyrimidin-2-yl)-3-azabicyclo[3.1.0]hexane-2-carboxylic acid (200 mg, 0.671 mmol), (6-(trifluoromethyl)-1H-indazol-4-yl)boronic acid (201 mg, 0.872 mmol), PdCl2(dppf) (49.1 mg, 0.067 mmol), and aqueous NaHCO3 (1.435 mL, 2.68 mmol) in dioxane (10 mL) to give an orange suspension. The vial was sealed and heated in a microwave reactor to 140° C. for 40 minutes. Additional (6-(trifluoromethyl)-1H-indazol-4-yl)boronic acid (201 mg, 0.872 mmol) and PdCl2(dppf) (49.1 mg, 0.067 mmol) were added and heating was continued for 45 minutes. The reaction mixture was subsequently partitioned between water (50 mL) and EtOAc (50 mL). The phases were separated. The organic layer was discarded and the aqueous layer was acidified with 1N HCl and extracted with EtOAc (2×75 mL). The organic layers were combined, washed with brine (50 mL), dried over Na2SO4, filtered, and concentrated to give the title compound as a tan glass, which was used without further purification (170 mg, 62.8%).

1. customto give an orange suspension
2. customThe vial was sealed
3. temperatureheating
4. customThe reaction mixture was subsequently partitioned between water (50 mL) and EtOAc (50 mL)
5. customThe phases were separated
6. extractionextracted with EtOAc (2×75 mL)
7. washwashed with brine (50 mL)
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated