Potassium Phosphate, Tribasic → HCID 58269022, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of compound 13g (14.3 mmol) in DMF (90 mL), was added 4,6-dichloropyrimidine (14.3 mmol), K3PO4, (42.7 mmol) and PCy3 (1.4 mmol) at rt. The mixture was purged with Ar for 45 min, Pd2(dba)3 (0.70 mmol) added and again the mixture purged with Ar for 30 min and heated to 100° C. for 1 h. The reaction was cooled to rt, EtOAc (800 mL) added, and the mixture filtered through Celite®. The combined filtrate was washed with water (3×200 mL), 2N aq. HCl solution (400 mL), sat. aq. NaHCO3 and brine solution (200 mL). The organic layer was dried (Na2SO4), filtered and concentrated to give a crude compound as a brown residue. The crude compound 7f was purified by column chromatography (100-200 mesh silica gel, 0-70% EtOAc/Petroleum ether). The product was obtained as a solid (350 mg, 10.6%). TLC system: EtOAc: Pet ether (7:3). Rf value: 0.56. mp: 260-270° C.

Provenance & Evidence