Step A: 5-methyl-1,3-benzodioxole (8.00 g, 58.8 mmol) was dissolved in chloroform (160 mL) and stirred under ice bath cooling. 60% nitric acid (20 mL) was slowly added dropwise to the reaction system, and after dropping, stirring was continued for 30 minutes at room temperature. After completion of the reaction, the reaction mixture was diluted with dichloromethane, washed sequentially with water and saturated sodium bicarbonate solution, and dried over anhydrous potassium carbonate. The desiccant was removed by filtration and the filtrate was concentrated under reduced pressure to give a light yellow solid 5-methyl-6-nitrobenzo[d][1,3]dioxole (9.58 g, 90% yield).1H-NMR (300 MHz, CDCl3) δ: 2.55 (s, 3H), 6.08 (s, 2H), 6.70 (s, 1H), 7.50 (s, 1H).
![5-Methyl-6-nitrobenzo[d][1,3]dioxole](/CAS/20150408/GIF/32996-27-3.gif)