Process for preparing solid amine oxides

A highly pure, white, solid amine oxide is prepared in high yield with minimal decomposition of the solvent by (A) reacting a tert-amine with a 15-20% stoichiometric excess of concentrated hydrogen peroxide at 50 DEG -55 DEG C. in the presence of controlled amounts of carbon dioxide and ethyl acetat...

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Bibliographische Detailangaben
Hauptverfasser: CHEN, Y.-D. MARK, WILSON, JR., R. WOODROW, SMITH, REBECCA F, MCGEE, SHARON B, KIM R, SHAH, MAYUR P
Format: Patent
Sprache:eng
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Zusammenfassung:A highly pure, white, solid amine oxide is prepared in high yield with minimal decomposition of the solvent by (A) reacting a tert-amine with a 15-20% stoichiometric excess of concentrated hydrogen peroxide at 50 DEG -55 DEG C. in the presence of controlled amounts of carbon dioxide and ethyl acetate until the reaction mixture contains 35-45 % by weight of ethyl acetate and less than 0.8% by weight of unreacted amine, (B) catalytically decomposing residual hydrogen peroxide, (C) separating the reaction mixture from the decomposition catalyst, (D) cooling the reaction mixture to 0 DEG C. to form a slurry, (E) centrifuging the slurry to separate the amine oxide, and (F) vacuum drying the amine oxide at ambient temperature-the reaction mixture being diluted to an amine oxide content of 25-30% by weight with additional ethyl acetate or a mixture thereof with a co-solvent, such as a low-boiling n-alkane, after the completion of Step A and prior to the beginning of Step D.