反应详情

温度

90 °C

To 0.22 g (1.00 mmol) biphenyl-4-yl-propynoic acid (I28) and 0.26 g (1.00 mmol) N-[2-(4-bromo-phenyl)-1-methyl-ethyl]-acetamide (I44.1) in 3.00 mL NMP are added 0.06 g (0.10 mmol) 1,1′-bis(diphenylphosphonino)ferrocene, 1.68 g (6.00 mmol) TBAF*H2O and 0.05 g (0.05 mmol) tris(dibenzylidenacetone)dipalladium(0). The reaction mixture is stirred at 90° C. for 3 h. The mixture is allowed to cool to r.t. and poured onto saturated aq NH4Cl solution. The precipitate is filtered, washed with water and purified by column chromatographie (silica gel; DCM/MeOH 9/1). The resulting product is triturated with isopropanol and dried at 60° C. in vacuo.

1. temperatureto cool to r.t.
2. filtrationThe precipitate is filtered
3. washwashed with water
4. custompurified by column chromatographie (silica gel; DCM/MeOH 9/1)
5. customThe resulting product is triturated with isopropanol
6. customdried at 60° C. in vacuo