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With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In toluene; for 10h;
35.144 mmol of 4-bromopyridine hydrochloride, 35.144 mmol, were weighed separately4-carboxyphenylboronic acid and 10 mmol of sodium carbonate were added to a toluene solution, and 0.08 mmol was addedOf tetraprophenylphosphonium palladium, in the catalyst tetrasthenyl phosphorus palladium under the action,Reaction for 10 h to obtain a white intermediate.The intermediate product is dried,Adding thionyl chloride,inReflux at 80 ° C,After completion of the reaction, the excess solvent was evaporated to dryness to give a yellow solid.The yellow solid was mixed with 5-aminoisophthalic acid in DMF and reacted at room temperature for 3 h. The reaction solution was added to 500 mL of distilled water,Precipitation of a large number of solid, that is, H2PYBI ligand.
With potassium carbonate;tetrakis(triphenylphosphine)palladium (0); In N-methyl-acetamide;
a 4-(4-pyridinyl)benzoic acid 4-Bromopyridine hydrochloride (0.4 g, 2 mmol), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoic acid (0.5 g, 2 mmol), and tetrakis(triphenylphosphine)palladium(0) (50 mg, 0.04 mmol) in dimethylformamide (15 mL) was treated with 2M potassium carbonate (2 mL) and the mixture was heated to 80° C. for 16 h. The mixture was concentrated in vacuo and the residue was diluted with water to afford a solid which was filtered to afford the title compound (0.26 g).
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