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A mixture of 3,5-dinitroaniline (12.8 g.) and acetic anhydride (64 ml.) was stirred during the dropwise addition of concentrated sulphuric acid (1.0 ml.). The temperature of the reaction mixture rose to about 45°C., and afer a few minutes colourless crystals were deposited. Afer 1 hour the reaction mixture was diluted with diethyl ether (200 ml.) and the crystalline solid was filtered off. Recrystallisation from a mixture of ethanol and water (2:1 by volume) gave 3',5'-dinitroacetanilide (11.5 g.) in the form of colourless plates, m.p. 191°-193°C.

1. customrose to about 45°C.
2. customafer a few minutes colourless crystals
3. filtrationthe crystalline solid was filtered off
4. customRecrystallisation
5. additionfrom a mixture of ethanol and water (2:1 by volume)