Ethanol → HCID 57855953, compound

Participants

Reaction Steps

To a suspension of 1 g (3.48 mmol) of 2,5-diamino-3-chloro-4-methylamino-benzoic acid methyl ester (synthesis described in example H7) in 153 ml of EtOH, is added 866 mg (6.97 mmol) of cyclopropane carboxamidine hydrochloride. After 24 hours of reaction under reflux, 866 mg (6.97 mmol) of cyclopropane carboxamidine hydrochloride were added more and the reaction is stirred under reflux 2 days more. Again 433 mg (3.48 mmol) of cyclopropane carboxamidine hydrochloride is added and after again 2 days of reaction under reflux, the reaction is stopped and the solvent is evaporated. The residue is suspended in EtOAc and the precipitate is filtrated. The filtrate obtained is evaporated and purified by flash chromatography on silica gel and gives 100 mg (0.36 mmol, 10%) of a brown solid. LC/MS: 280/282 (M+1)+

Provenance & Evidence