Hydrochloric Acid → HCID 19434854, compound

Participants

Reaction Steps

340 mg (0.594 mmol) of the above 6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-7-(4-methylpiperazin-1-yl)-5-pivaloylamino-4H-1-benzopyran-4-one was dissolved in 20 mL of 1,4-dioxane, 10 mL of concentrated hydrochloric acid was added and the mixture was heated at reflux for 2.5 hours. The reaction solution was cooled on ice, adjusted to pH 10 and extracted twice with chloroform (containing a small amount of methanol). The organic layer was washed once with an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=12:1) to give 117 mg of Compound 98 (yield: 49%).

Provenance & Evidence