Methanesulfonic Acid → HCID 178433898, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of methanesulfonic acid (30 mL) and phosphorus pentoxide (6 g) was heated at 100° C. The mixture was stirred thoroughly at the temperature, with gradual addition of powdery ethyl 2-benzoyl-3-[[3-methyl-1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]-2-propenoate (3.0 g, 8.0 mmol). The mixture was further heated and stirred at the temperature for 30 minutes. The solution was cooled to room temperature, iced water was added thereto. The solution was neutralized by the addition of an aqueous sodium hydroxide solution, and organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Purification of the residue by basic silica gel column chromatography (chloroform) gave the title compound (880 mg, 34% yield).

Provenance & Evidence