Aim To prepare and submit picric acid

Reference : Mann & saunders, “practical organic chemistry” fourth

edition, published by pearsns pvt ltd, pg no. 170-174
Required: Phenol, 8 g.; sulphuric acid, 10 ml.; nitric acid 30 ml.

 Weigh out 8 g. of phenol into a dry 750 ml. flat-bottomed flask,

 Add 10 ml. (18-5 g.) of concentrated sulphuric acid, and
 Shake the mixture, which becomes warm.
 Heat the flask on a briskly boiling water-bath for 30 minutes to
complete the formation of the phenol-sulphonic acid.
 Then chill the flask thoroughly in an ice-water mixture.
 Place the flask on a wooden block (or on some similar non-
conducting surface) in an efficient fume-cupboard, and without
delay, i.e., whilst the phenolsulphonic acid is still a cold viscous
syrup,
 Add 30 ml. of concentrated nitric acid and at once thoroughly mix
the liquids by shaking for a few seconds.
 Then allow the mixture to stand undisturbed.
 Usually within one minute a vigorous (but harmless) reaction
occurs,
 Red fumes pour out of the flask.
 When the action subsides, heat the flask on a boiling water-bath for
1 hours, with occasional shaking.
 During this period the heavy oil, which is present at the beginning,
ultimately forms a mass of crystals.
 When the heating is complete, add ioo ml. of cold water, mix well
and then chill thoroughly in ice-water.
 Filter the yellow crystals at the pump, wash thoroughly with water
to eliminate all inorganic acid and drain.
  Recrystallise from a mixture of I volume of ethanol and 2 volumes
of water, about 90 ml. of the mixed solvent being required.
 Picric acid is obtained in pale yellow leaflets, m.p. 122°,
 Dry by pressing between sheets of drying-paper, or in a desiccator.

Yield of recrystallised material:……………………………………….