Synthesis of Bis(2,4-dinitrophenyl)oxalate (DNPO)

A 3-neck RBF equipped with a thermometer, a rubber septum, and a drying tube is set up and immersed in an ice bath. 18.4 g of dry 2,4-dinitrophenol is dissolved in 250 mL of dry toluene in the RBF, and an addition of 10.1 g of triethylamine is started over the course of 5 minutes with stirring. Then the drying tube is replaced with an addition funnel filled with 7 g of oxalyl chloride dissolved in 30 mL of dry toluene. A slow addition of the solution is started with vigorous stirring whilst maintaining the temperature below 10°C. After which the mixture is let to stand at room temperature for 12h and then filtered. The crude product is then transferred to a beaker and combined with 50 mL of chloroform, the mixture is then filtered and the pure product is dried in open air.

Source

The toluene solution

Addition of the triethylamine

Addition of the oxalyl chloride

The mixture after addition

The crude product

Combining the product with chloroform

Filtration

The dried pure product

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