Process for the preparation of a very pure commercial form...

Details Process for the preparation of a very pure commercial form... Process for the preparation of a very pure commercial form...

C - Chemistry, Metallurgy

07

C

260/619.3

C07C 41/34 (2006.01) C07C 41/26 (2006.01) C07C 43/295 (2006.01)

Patent

CA 1246097

Process for the preparation of a very pure commercial form of 4,2',4'-trichloro-2-hydroxydiphenyl ether Abstract A very pure, dust-free commercial form of 4,2',4'- trichloro-2-hydroxydiphenyl ether with little odour is pre- pared by diazotising 4,2',4'-trichloro-2-aminodiphenyl ether, boiling the diazonium salt and purifying the reaction product. The pure, dust-free and odour-free commercial form is obtained by separating off the acid aqueous phase of the reaction mixture, rendering the mixture containing 4,2',4'-trichloro-2-hydroxydiphenyl ether and 2,4,8-tri- chlorodibenzofuran alkaline, extracting it several times with an inert water-immiscible solvent, either after removal of the organic solvent by steam distillation and precipi- tation of the by-product 2,4,8-trichlorodibenzofuran or directly, and then adjusting the pH to 3 to 10; subsequently, the highly volatile constituents are removed from the 4,2',4'-trichloro-2-hydroxydiphenyl ether melt which has separated out, the melt is subjected to molecular distil- lation and the distilled melt is introduced into an aqueous dispersion of crystalline 4,2',4'-trichloro-2-hydroxydipheny ether, this dispersion simultaneously being subjected to wet grinding. Filtration and drying gives a granular-like ready- to-use commercial form.

421179

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