In a
2-l. round-bottomed flask equipped with an
efficient mechanical stirrer (Note
1) are placed
110 g. (0.4 mole) of freshly prepared, pulverized iodobenzene dichloride (p. 482) (Note
2),
1.0 mole of sodium hypochlorite solution (Note
3), and
2 ml. of glacial acetic acid. The vigorously stirred mixture is heated on a
water bath maintained at 65–75°. After 10–15 minutes the heated mixture becomes frothy and the yellow color of
iodobenzene dichloride is displaced by the white color of
iodoxybenzene. The stirring is stopped after 1 hour, and the flask is cooled in an
ice bath. The product is filtered with suction, pressed with a
glass stopper, and transferred to an
800-ml. beaker. The material is stirred thoroughly with 300 ml. of water, filtered with suction, washed on the filter with 100 ml. of water, pressed, and dried in the air. The crude product weighs
85–89 g. (
90–94%) and has a purity, as determined iodimetrically, of 97–99% (Note
4). The air-dried material may be washed with
50–60 ml. of chloroform, air-dried, and finally dried in a
vacuum desiccator. This product weighs
82–87g. (
87–92%) and has a purity of 99.0–99.9% as determined by iodimetry (Note
5).