Methane → HCID 20475065, compound

Participants

Reaction Steps

A mixture of 5.5 g (0.0201 mol) of 11-chlorocarbonyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 6.9 g (0.06 mol) of 1-amino-4-methylpiperazine and 150 ml of anhydrous dioxane was heated for 30 minutes over a steam bath and the cloudy reaction mixture obtained was then mixed while still hot with 2 g of active charcoal, then filtered and the filtrate obtained was concentrated by evaporation in vacuo. The residue was purified by column chromatography on 300 g of silica gel, using a mixture of dichloromethane, methanol and conc. aqueous ammonia (ratio by volume 800:200:5). The residue remaining after the eluates of interest had been evaporated was recrystallized from ethanol. 1.5 g (19% of theory) of colorless crystals of 5,11-dihydro-11-[[(4-methyl-1-piperazinyl)amino]-carbonyl]-6H-pyrido[2,3-b]-[1,4]benzodiazepin-6-one hydrochloride hydrate was obtained,

Provenance & Evidence