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

5-Methyl-1,3-benzodioxole (8.00 g, 58.8 mmol) was dissolved in chloroform (160 ml), and the mixture was stirred under ice-cooling. To this solution was gradually added 60% nitric acid (20 ml), and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with dichloromethane, washed with water and saturated aqueous sodium hydrogen carbonate, and dried over potassium carbonate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give the title compound (9.58 g, yield 90%) as a pale-yellow solid.

1. temperaturecooling
2. stirringthe mixture was stirred at room temperature for 30 min
3. washwashed with water and saturated aqueous sodium hydrogen carbonate
4. dry with materialdried over potassium carbonate
5. filtrationThe insoluble material was filtered off
6. concentrationthe solution was concentrated under reduced pressure

ORD record

ord-d622537d0d57496f8d10b97bbaadf49d

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08513235B2