p-Toluenesulfonic acid → HCID 70109536, compound

Participants

Reaction Steps

Methyl p-aminophenylacetate (7 g), ethyl trifluoroacetoacetate (8.19 g) and p-toluenesulfonic acid (500 mg) were dissolved into benzene (100 ml) and, providing Dean Stalk dehydrating apparatus placed molecular sieve (MS 4 angstroms) therein, the solution was refluxed for 10 hours under heat. Solvent was distilled off under reduced pressure and the residue was purified by means of silica gel column chromatography (development solvent: ethyl acetate:hexane=1:4) to obtain methyl 3-(4-methoxycarbonylmethylphenylamino)-3-trifluoromethylacrylate (7.18 g) as colorless prismatic crystals. Melting point: 50°-51° C. (recrystallization solvent: ethyl acetate-n-hexane)

Provenance & Evidence