In a
large mortar chilled in an
ice bath are placed
55 g. (0.2 mole) of iodobenzene dichloride (p. 482),
50 g. of anhydrous sodium carbonate, and 100 g. of finely crushed ice. The mixture is ground thoroughly (Note
1) until all the ice has melted and a thick paste results. To this suspension
140 ml. of 5 N sodium hydroxide is added, in 20-ml. portions, with repeated trituration after each addition. Finally, 100 ml. of water is added to render the mixture more fluid and the material is allowed to stand overnight. The product is collected with suction, pressed thoroughly on the filter, transferred to a
beaker, and washed thoroughly with 300 ml. of water (Note
2). The material is filtered with suction, washed again in a beaker with 300 ml. of water, collected with suction, and washed with about 250 ml. of water on the filter. After thorough drying in the air, the product is stirred to a thin mush with a little
chloroform (Note
3), freed of solvent by suction, and spread on filter paper to dry in the air. The yield is
26–27 g. (
60–62%) of a product having a purity of about 99%, as determined by titration (Note
4) and (Note
5).