Hydrazine hydrate (1:1) → HCID 9840673, compound

Participants

Reaction Steps

0.1 g of Raney nickel and 0.25 ml (4.93 mmol) of 98% hydrazine hydrate are added to a suspension of 0.6 g (1.64 mmol) of 7-acetyl-5-(4-nitrophenyl)-8-methyl-7H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine in 40 ml of methanol. The mixture is stirred for 0.5 hour. The starting material is dissolved within a few minutes. After the reaction is completed, catalyst is filtered out. The filtrate is concentrated by evaporation in a vacuum. The residue is absorptively precipitated in water, suctioned off and rewashed with water. 0.49 g of 7-acetyl-5-(4-aminophenyl)-8-methyl-7H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine with a melting point of 175°-180° C. is obtained. Recrystallization of this crude product from 50% aqueous ethanol yields 0.46 g (79%) of 7-acetyl-5-(4-amino-phenyl)-8-methyl-7H-1,3-dioxolo[4,5-h][2,3]-benzodiazepine with a melting point of 208°-210° C.

Provenance & Evidence