60 mL of white fuming nitric acid is cooled down in an ice bath, then a slow addition of 11g of mannitol is started with vigorous stirring. The temperature must be kept below 0°C. Thereafter a slow addition of 80 mL of conc. sulfuric acid is started with stirring, manual stirring may be required as the reaction proceeds. The mixture is then poured into 800 mL of cold water, the mixture is filtered and washed with sodium carbonate solution and water. The crude product is then recrystallized from hot methanol.
The mixture after the addition of the mannitol
Addition of the sulfuric acid
The crude product in water
Filtration and washing
The crude product