反应详情

24 ml of nitric acid (d=1.4) in 60 ml of glacial acetic acid were added dropwise at 15°-20° C. to 39.0 g of 2,2-dimethyl-1,3-benzodioxole in 200 ml of glacial acetic acid. After stirring at room temperature for 3 hours, the mixture was poured into ice/water and extracted twice with 1 l of methylene chloride. The organic phase was washed neutral with water, dried over sodium sulfate and evaporated in vacuo. The residue, recrystallized from methanol, gave 17.0 g (33.5% of theory) of 2,2-dimethyl-5-nitro-1,3-benzodioxole of melting point 88°-90° C.

1. extractionextracted twice with 1 l of methylene chloride
2. washThe organic phase was washed neutral with water
3. dry with materialdried over sodium sulfate
4. customevaporated in vacuo
5. customThe residue, recrystallized from methanol