反应详情

温度

80 °C

A mixture of 2-(4-bromo-2,6-difluorobenzylthio)-5-(2-(4-chloro-3-methoxyphenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazole (0.79 g, 1.35 mmol), propargyl alcohol (122 μL, 2.03 mmol), pyrrolidine (169 μL, 2.03 mmol), CuI (26 mg, 0.13 mmol) and PdCl2(dppf)2 (50 mg, 0.07 mmol) in DMF (6.80 mL) was purged with argon and then heated to 80° C. for 3 h. The reaction mixture was filtered through Celite™ to remove solids. The filter agent was rinsed with EtOAc (3×75 mL). The filtrate was washed with water and brine, dried over anhyd Na2SO4, concentrated and purified by flash chromatography (80% EtOAc/Hex) to give the title compound (714 mg, 94%) as a yellow solid. MS (EI) m/z 557 (MH+).

1. customwas purged with argon
2. filtrationThe reaction mixture was filtered through Celite™
3. customto remove solids
4. washThe filter agent was rinsed with EtOAc (3×75 mL)
5. washThe filtrate was washed with water and brine
6. dry with materialdried over anhyd Na2SO4
7. concentrationconcentrated
8. custompurified by flash chromatography (80% EtOAc/Hex)