Process for preparing storage-stable benzothiazolyl sulfenamides

本发明提供一种在过氧化氢和碱金属次氯酸盐存在下,使伯胺与巯基苯并噻唑的碱金属盐反应制备苯并噻唑基亚磺酰胺的方法。本发明的方法特征在于高转化率,其中得到的苯并噻唑基亚磺酰胺具有高纯度、高产率、即使在高温和高湿度下也具有高储存稳定性。 A process for the production of benzothiazolyl sulfenamides by reaction of a primary amine and alkali metal salts of mercaptobenzothiazole in the presence of hydrogen peroxide dosed in...

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1. Verfasser: SLUYTS DOMIEN,FELIX LEON,PREUSS REINHARD,MISSIAEN PATRICK,GRABOWSKI STEFAN
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creator SLUYTS DOMIEN,FELIX LEON,PREUSS REINHARD,MISSIAEN PATRICK,GRABOWSKI STEFAN
description 本发明提供一种在过氧化氢和碱金属次氯酸盐存在下,使伯胺与巯基苯并噻唑的碱金属盐反应制备苯并噻唑基亚磺酰胺的方法。本发明的方法特征在于高转化率,其中得到的苯并噻唑基亚磺酰胺具有高纯度、高产率、即使在高温和高湿度下也具有高储存稳定性。 A process for the production of benzothiazolyl sulfenamides by reaction of a primary amine and alkali metal salts of mercaptobenzothiazole in the presence of hydrogen peroxide dosed in over a period greater than or equal to 2 hours followed by the addition of the alkali metal hypochlorite over an at least 10 minute period and adjustment of the pH to 11.5-12 at the end of the reaction. A process for the production of benzothiazolyl sulfenamides (I) by reaction of a primary amine with alkali metal salts of mercaptobenzothiazole in the presence of hydrogen peroxide and alkali metal hypochlorites comprises reaction of an aqueous solution of a metal salt of mercaptobenzothiazole with the primary amine in the presence of up to 90 mol.% hydrogen peroxide (with respect to the mercaptobenzothiazole) at pH 10.0-11.0 whereby the hydrogen peroxide is dosed in over a period greater than or equal to 2 hours followed by the addition of the alkali metal hypochlorite over an at least 10 minute period and adjustment of the pH to 11.5-12 at the end of the reaction whereby the amount of primary amine added is 100-500 mol.% and the sum of hydrogen peroxide and alkali metal hypochlorite added is up to 130 mol.% (with respect to the amount of the alkali metal salt of the mercaptobenzthiazole).
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METALLURGY
ORGANIC CHEMISTRY
title Process for preparing storage-stable benzothiazolyl sulfenamides
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