Method for making dimethyl sulfone from dimethyl sulfoxide and hydrogen peroxide
First Claim
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1. A method for making crystalline dimethyl sulfone comprising:
- (a) simultaneously adding dimethyl sulfoxide and an aqueous solution of hydrogen peroxide to a preheated, stainless steel reaction vessel precharged with an aqueous solution of dimethyl sulfone at a rate sufficient to maintain the reaction temperature below about 120°
C.;
(b) distilling water from the reaction mixture;
(c) adding water to the reaction mixture to form a dilute reaction solution;
(d) heating and filtering the heated reaction solution;
(e) cooling the reaction solution to crystallize out the dimethyl sulfone; and
(f) filtering or centrifuging the crystallized dimethyl sulfone.
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Abstract
The present invention provides a process for synthesizing dimethyl sulfone by the oxidation of dimethyl sulfoxide with hydrogen peroxide.
5 Citations
23 Claims
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1. A method for making crystalline dimethyl sulfone comprising:
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(a) simultaneously adding dimethyl sulfoxide and an aqueous solution of hydrogen peroxide to a preheated, stainless steel reaction vessel precharged with an aqueous solution of dimethyl sulfone at a rate sufficient to maintain the reaction temperature below about 120°
C.;
(b) distilling water from the reaction mixture;
(c) adding water to the reaction mixture to form a dilute reaction solution;
(d) heating and filtering the heated reaction solution;
(e) cooling the reaction solution to crystallize out the dimethyl sulfone; and
(f) filtering or centrifuging the crystallized dimethyl sulfone. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11)
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12. A method for making flaked dimethyl sulfone comprising:
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(a) simultaneously adding dimethyl sulfoxide and an aqueous solution of hydrogen peroxide to a preheated, stainless steel reaction vessel precharged with an aqueous solution of dimethyl sulfone at a rate sufficient to maintain the reaction temperature below about 120°
C.;
(b) distilling water from the reaction mixture;
(c) cooling the reaction mixture to below 80°
C.;
(d) adjusting the pH of the reaction mixture to about between 8 and 9;
(e) distilling water and forerun from the reaction mixture at atmospheric pressure followed by vacuum of at least 40 mm Hg and then followed by vaccum of 20-30 mm Hg. (f) distilling the product at about 160-175°
C. as a colorless oil that solidifies upon cooling; and
(g) flaking the product to provide a flowable material. - View Dependent Claims (13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23)
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Specification