Diphenyliodonium IODATE

The interaction of iodosobenzene and iodoxybenzene in the presence of aqueous sodium hydroxide yields the soluble diphenyliodonium iodate (IV) upon adding potassium iodide solution, the sparingly soluble diphenyliodonium iodide (V), analogous to ammonium iodide is precipitated ... 

Grind together 12 g (0.05 mol) of iodylbenzene (Expt 6.33), and 11 g (0.05 mol) of iodosylbenzene (Expt 6.32) with 25 ml of water, add 100 ml of 1 m sodium hydroxide solution and stir for 24 hours in a 1-litre vessel. Dilute with 500ml of cold water, stir thoroughly, allow to settle and decant the supernatant solution of diphenyliodonium iodate, through a fluted filter paper. Extract the solid residue with two 250 ml portions of water, and decant the extract... 

Preparation. A mixture of benzene, potassium iodate, sulfuric acid, and acetic anhydride is stirred until reaction is complete and then diluted with water. Extraction with ether and treatment with aqueous ammonium chloride gives a precipitate of diphenyliodonium chloride in yield of 63%. 

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