Nitric Acid → 5,6-Dinitro-1,3-benzodioxole

Participants

Reaction Conditions

Reaction Steps

0.103 mol (17.2g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), tne temperature being maintained at between 0° C. and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice; the expected product pre,ipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C. -100° C.). It can optionally be recrystallized from 96° strength ethanol.

Provenance & Evidence