To a cooled flask immersed in an ice bath is added 100 mL of very cold conc. nitric acid and 200 mL of very cold 95% sulfuric acid, to the mixture slowly, with stirring, is added 60 g of nitroisobutylglycerol. The temperature should be maintained at 0-10°C. The mixture is stirred for additional 15 minutes and then cooled down in a freezer to separate the 2 layers. The upper acid layer is decanted and the bottom organic layer is washed twice with saturated sodium carbonate solution. No shaking should be applied in the washing steps since emulsion is formed. The organic layer is then dried over anhydrous magnesium sulfate and stored under the presence of an inert gas in a freezer.
The cold nitration solution
Addition of the NIBG
The NIBG hardly dissolves at first but slowly starts to form the nitrated oily product
The oily NIBGTN layer at the bottom
The pure product