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With sodium carbonate;palladium diacetate; triphenylphosphine; In propan-1-ol; for 2.5h;Heating / reflux;
Preparation 114: 5-(2-Fluoro-6-methyl-pyridin-3-yl)-2,4-dimethoxy-pyrimidine (Prep114); 2,4-Dimethoxy-pyrimidine-5-boronic acid (1.16 g, 6.32 mmol) was dissolved in degassed n-PrOH (22 ml) and then <strong>[884494-48-8]2-fluoro-6-methyl-3-iodopyridine</strong> (870 mg, 3.67 mmol), Na2CO3 (778 mg, 7.34 mmol), PPh3 (96 mg, 0.37 mmol) and Pd(OAc)2 (41 mg added in three portions) were added. The suspension was stirred at reflux for 2.5 hours. The solvent was evaporated under vacuum and the crude was partitioned between water and DCM. The organic phase was dried (Na2SO4) and evaporated. The crude was triturated with iPrOH to give 691 mg of the title compound (75% yield). MS (ES) (mlz): 250.1 [M+H]+.
With triethylamine;copper(l) iodide; tetrakis(triphenylphosphine) palladium(0); at 90℃; for 2.0h;
A solution of Compound 1c (23 mg; 0.946 mmol), Reagent B (0.253 mmol), tetrakis(triphenylphosphine)palladium(0) (8 mg, 0.0069 mmol) and copper(I) iodide (2 mg, 0.0105 mmol) in triethylamine (4 mL), in a sealed vessel, was stirred at 90 C. for 2 h, cooled to r.t., poured into water and extracted with EtOAc. The EtOAc solution was washed with water, dried over Na2SO4 and evaporated to dryness in vacuo. Purification by flash chromatography (EtOAc-ETP 2:8), afforded the title products.