Sulfuric Acid → HCID 9817233, compound

Participants

Reaction Conditions

Reaction Steps

To 3-ethyl-4-(4-methylisoxazol-5-yl)-5-(methylthio)thiophene-2-carbonitrile (0.87 g, 3.3 mmol) was added conc. sulfuric acid (11 ml) and the mixture was heated at 60° C. for 1.5 hours. The reaction solution was allowed to cool down to room temperature, ice was added and then the mixture was extracted with ethyl acetate. The organic layer was washed (with water, saturated aqueous sodium hydrogen-carbonate and saturated aqueous sodium chloride, in turn), dried (over anhydrous magnesium sulfate) and concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (developing solvent: chloroform/ ethyl acetate=1:0-3:1) and recrystallized from diethyl ether to afford 3-ethyl-4-(4-methylisoxazol-5-yl)-5-(methylthio)thiophene-2-carboxamide (0.39 g, 42%) as colorless crystals.

Provenance & Evidence