4-Cyanobenzoyl chloride → HCID 19921297, compound

Participants

Reaction Conditions

Reaction Steps

48.6 g of 3-amino-4-(3-thiomorpholino-propylamino)-benzoic acid-[N-(2-methoxycarbonyl-ethyl)-amide]-hydrochloride are dissolved in 500 ml of glacial acetic acid with heating, 19.5 g of 4-cyano-benzoylchloride are added, the mixture is heated for one hour over a steam bath and a further 2 hours at a bath temperature of 120° C. The mixture is evaporated down in vacuo and the residue is purified by chromatography on silica gel (eluant:methylene chloride/methanol/conc. ammonia=9:1:0 to 8:2:0.2). Yield: 33.7 g (58% of theory), Rf value: 0.84 (silica gel; methylene chloride/methanol/conc. ammonia=19:1:0.1, after developing three times)

Provenance & Evidence