- Preparation method of aromatic sulfonic acid compound
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The invention discloses a preparation method of an aromatic sulfonic acid compound, and aims to provide the preparation method of the aromatic sulfonic acid compound, wherein the method is simple in process, low in equipment requirements, high in capacity, wide in raw material sources and small in environmental influence. The method is characterized by comprising the steps: with a starting material aromatic amine compound, dissolving in an acid, carrying out a diazotization reaction with sodium nitrite to prepare a diazocompound; carrying out a reaction of a catalyst cuprous salt with a thionyl chloride aqueous solution, and carrying out a sulfonylation reaction with the prepared diazocompound to obtain an aromatic sulfonyl chloride compound or an aromatic sulfonyl chloride hydrochloride compound, next hydrolyzing to obtain a crude product aromatic sulfonic acid compound, finally purifying through a beating way by an acidic solvent and an alcohol solution, and thus obtaining the high-purity aromatic sulfonic acid compound. The method is friendly to environment, has certain cost advantages, avoids use of more expensive aromatic thiol compounds as starting materials, and is beneficial for industrial production.
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Paragraph 0021; 0022
(2016/11/17)
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- Aqueous process chemistry: The preparation of aryl sulfonyl chlorides
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The use of aqueous acidic conditions for the preparation of arylsulfonyl chlorides from diazonium salts in the presence of copper salts, preferably CuCl, together with thionyl chloride as the sulfur dioxide source, has considerable advantages over recommended literature procedures, whereby reactions are carried out in acetic acid with minimisation of water content of the solvent. The method has been shown to be successful for a wide range of electron-deficient and electron-neutral aryl substrates. The sulfonyl chlorides are protected from hydrolysis by their low solubility in water, which results in their direct precipitation from the reaction mixture in good yields (>70%) and high strength (>98% w/w). The aqueous process, which is additionally safer and more robust, can be readily scaled up and has significant environmental benefits.
- Hogan, Philip J.,Cox, Brian G.
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scheme or table
p. 875 - 879
(2010/04/22)
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