Nitric Acid → 5-Methyl-6-nitro-1,3-benzodioxole

Participants

Reaction Steps

To a solution of 10 (19.0 g, 139.6 mmol) in acetic acid (180 mL) was added a solution of fuming HNO3 (10 mL) in acetic acid (70 mL) dropwise over 30 minutes. The mixture was stirred at ambient temperature for 10 minutes, then poured into a beaker containing ice to give a crystalline precipitate, which was collected by vacuum filtration and washed with water to afford the crude product. Further purification via recrystallization from CH2Cl2/hexane gave the pure product (16.3 g, 64.4%).

Provenance & Evidence