Sodium Azide → HCID 178423506, compound

Participants

Reaction Steps

To a solution of 15 g of 5-methyl-2,6-dihydrodibenzo[cd,g]indazol-6-one prepared in Example 25-b in 70 ml concentrated sulfuric acid was added 12.5 g of sodium azide [CAS No. 26628-22-8], followed by stirring at room temperature for 30 hours. The reaction mixture was poured onto 700 ml of ice-water, the precipitated powder was collected by filtration and dried in vacuo. The resulting powder was dissolved in a solvent mixture of dimethylformamide-ethyl acetate, sequentially washed with saturated aqueous sodium hydrogencarbonate solution and brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was recrystallized from dimethylformamide-ethyl acetate, to give 6.59 g of the title compound as ocher yellow crystals.

Provenance & Evidence