Into a large round-bottomed flask prepare a mixture of 107 g of 3-nitroaniline and 1000 mL of concentrated (>96%) sulfuric acid.  Heat the mixture to 60 C and remove the heat source.  Very slowly add, dropwise, 190 mL of 100% nitric acid.  The rate of acid addition is done at such a rate as to keep the temperature between 62 and 68 C.  An external cooling bath may help.  After the addition is complete stir the mixture for 20 minutes with no heating or cooling.  An ice bath is now used to quickly drop the temperature to 40 C.  The mixture is poured over a fritted glass filter to collect the precipitated product.  The crystals are washed with 50% sulfuric acid, then with water, and they are left to dry on the disk.  Yield is about 157 g or 74% of damp tetranitroaniline.

* The boiling point of this compound is only theoretical, not an experimentally determined value. Explosives rarely reach their boiling point at the standard state before detonating or igniting.

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