Nitric Acid → HCID 67452110, compound

Participants

Reaction Conditions

Reaction Steps

50 g ((2-(2-(2-(Bis-methoxycarbonylmethyl-amino)-phenoxy)-ethoxy)-4-methyl-phenyl)-methoxycabonylmethyl-amino)-acetic acid methyl ester were dissolved in 600 ml glacial acetic acid. Under vigorous stirring 91.5 ml 1 molar nitric acid in glacial acetic acid was added and in a second step 28 ml of concentrated sulfuric acid was added. The temperature increased up to 30° C. The reaction mixture was directly poured in a 10 l ice/water mixture. The residue was filtered off, washed several times with water and dried under vacuum. The crude product was further purified by column chromatography on silica gel first with hexane/acetic acid ethyl ester (1:1) as eluent and a second time with toluene/acetonitrile (1:1) as eluent. The product was finally crystallized from propan-2-ol. Yield: 20 g.

Provenance & Evidence