* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; water; at 110.0℃;Inert atmosphere;
General procedure: E1 (1.00 equivalents), E2 (1 .15 equivalents), Pd(dppf)Cl2 (0.05 equivalents) and potassium acetate (2.50 equivalents) are stirred under nitrogen atmosphere in a mixture of dioxane and water (10:1 ) at 1 10 C until completion of the reaction (monitoring with GC/MS, usually finished within 4-24 h). Active carbon and Celite are added to the reaction mixture and stirred at 100 C for 10 minutes. Subsequently, the mixture is hot filtered and concentrated under reduced pressure. The residue is dissolved in dichloromethane and washed with water and brine. The organic phase is dried with MgS04, filtrated and reduced under reduced pressure. The obtained crude product is purified via recrystallization using toluene as solvent, giving E3 as solid.
59%
With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In 1,4-dioxane; water; at 110.0℃;Inert atmosphere;
E1 (1.00 equivalents), E2 (1 .15 equivalents), Pd(dppf)Cl2 (0.05 equivalents) and potassium acetate (2.50 equivalents) are stirred under nitrogen atmosphere in a mixture of dioxane and water (10: 1 ) at 1 10 C until completion of the reaction (monitoring with GC/MS, usually finished within 4-24 h). Active carbon and Celite are added to the reaction mixture and stirred at 100 C for 10 minutes. Subsequently, the mixture is hot filtered and concentrated under reduced pressure. The residue is dissolved in dichloromethane and washed with water and brine. The organic phase is dried with MgS04, filtrated and reduced under reduced pressure. The obtained crude product is purified via recrystallization using toluene as solvent, yielding E3 as a solid. AAV2 (59% yield), wherein 4-chloro-2,6-diphenylpyrimidine (CAS 29509-91-9) was used as reactant.