HCID 18183116, compound → HCID 18183117, compound

Participants

Reaction Steps

834 mg of 2,3-dimethyl-8-methoxy-6-(4-nitrophenyl)-11H-imidazo[1,2-c][2,3]benzodiazepine in 33 ml of glacial acetic acid together with 2.25 g of iron powder are heated for 20 minutes in an oil bath that is preheated to 90° C. It is suctioned off hot and rewashed with glacial acetic acid. The filtrate is concentrated by evaporation, and the residue is dispersed in ethyl acetate and 1N sodium hydroxide solution. The aqueous phase is shaken out twice with ethyl acetate, and the collected organic phase is washed with water, dried, filtered and concentrated by evaporation. This residue is chromatographed on silica gel with methylene chloride:ethanol=10:1 as an eluant. After the corresponding fractions that are concentrated by evaporation are absorptively precipitated with ethyl acetate/hexane, 331 mg of 6-(4-aminophenyl)-2,3-dimethyl-8-methoxy-11H-imidazo[1,2-c][2,3]benzodiazepine with a melting point of 280° C. is obtained.

Provenance & Evidence