Potassium Carbonate → 1-(2,6-Dichlorophenyl)-5-(2,4-difluorophenyl)-3,4-dihydro-7-hydroxy-2(1H)-quinolinone

Participants

Reaction Steps

The mixture of compound 1 (126 mg, 0.3 mmol) and sodium hydride (60%) (12 mg, 0.3 mmol) in 6 mL of DMF was stirred for 1 h at rt. Then the compound 2 (78 mg, 0.33 mmol) was added and stirred for 12 h at 135° C. Potassium carbonate (83 mg, 0.6 mmol) and compound 2 (78 mg, 0.33 mmol) was again added to the reaction mixture and stirred for another 24 h at 135° C. After removal of solvent, it was poured in to 30 mL of ethyl acetate and 10 mL of aq Na2CO3, and it was extracted with ethyl acetate (15 mL×3). The combined organic layer was dried over Na2CO3 and concentrated. After removal of solvent, the residue was purified by TLC with hexane/ethyl acetate/2N NH3 in MeOH to afford compound 3 (white solid). Mass spectrum (ESI) for 3, 555 (M+1) and 557 (M+3).

Provenance & Evidence