p-Nitrobenzoyl peroxide (CAS NO.: ), with other names as Peroxide, bis(p-nitrobenzoyl), could be produced through the following synthetic routes.

A 600-ml. beaker containing 100 ml. of water and equipped with an efficient stirrer, a thermometer, and a 200-ml. separatory funnel is immersed in an ice-water bath. When the temperature of the water has fallen to 0–5°, 10 g. (0.13 mole) of sodium peroxide is added. Then, with vigorous stirring, a solution of 37 g. (0.2 mole) of p-nitrobenzoyl chloride in 100 ml. of dry toluene is added dropwise over a period of about 30 minutes. After the mixture has been stirred for an additional 1.5 hours, the precipitate is filtered and washed with 200 ml. of cold water. The yield of p-nitrobenzoyl peroxide is 28.5–29 g. (86–88%). It melts at 155–156°.

The product may be recrystallized most conveniently by dissolving it as rapidly as possible in 500 ml. of dry toluene which has been preheated to 80–85°. As soon as the solid is completely dissolved (2–3 minutes of stirring), the solution is filtered through a warm Büchner funnel and the filtrate is immediately cooled in an ice-water bath. The yield of very pale yellow glistening needles is 25 to 26 g. (86–89% recovery); they melt at 156° with vigorous decomposition.