Potassium Phosphate, Tribasic → HCID 86684040, compound

Participants

Reaction Conditions

Reaction Steps

A 100-mL round-bottomed flask equipped with a reflux condenser was charged with 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-4-chloronicotinaldehyde 103b (150 mg, 0.42 mmol), 148d (278 mg, 0.63 mmol), Pd(dppf)Cl2 (17.1 mg, 0.021 mmol), K3PO4 (178.1 mg, 0.84 mmol), sodium acetate (68.9 mg, 0.84 mmol), acetonitrile (15 mL), and water (5 drops). The system was subjected to three cycles of vacuum/nitrogen flush and heated at 100° C. under N2 protection for 1 h. Analysis of the reaction mixture by LCMS showed complete conversion to the desired product. It was cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure. The residue was washed with acetonitrile (0.5 mL) to afford 148e as a white solid (100 mg, 37%), which was used in the next step without further purification. MS-ESI: [M+H]+ 638.8

Provenance & Evidence