Preparation of esters
    1.
    发明公开
    Preparation of esters 失效
    Verfahren zur Herstellung von Estern。

    公开(公告)号:EP0294073A1

    公开(公告)日:1988-12-07

    申请号:EP88304690.6

    申请日:1988-05-24

    IPC分类号: C07C309/58

    CPC分类号: C07C309/00

    摘要: Hitherto processes proposed in recent years for preparing esters of phenol sulphonate salts by reaction between a carboxylic acid chloride and a phenol sulphonate salt place considerable emphasis upon dehydrating the reactants before they are brought into contact in an organic solvent reaction medium.
    The present invention avoids the problems of employing non-aqueous solvents by carrying out the reaction under aqueous conditions but with controlled alkalinity and water content, especially at a base to phenol sulphonate mole ratio of from 1.3:1 to 1.6:1 and a total water to phenol sulphonate (as the anhydrous material) of not more than 4.5:1. The reaction advantageously employs in preference only a small molar excess of carboxylic acid chloride over the phenol sulphonate and preferably has a reaction temperature controlled to below 30°C, especially 5 to 20°C.
    In a further improvement to the process, the difficulty of enhanced contamination with benzoic acid in the products can be ameliorated by employing a small but effective amount of a surfactant, especially an alcohol ethoxylate, in the reaction mixture.
    The process is especially well suited to making sodium benzoyl oxybenzene sulphonate from sodium phenol sulphonate dihydrate and benzoyl chloride.

    摘要翻译: 迄今为止,通过羧酸酰氯和苯酚磺酸盐之间的反应制备苯酚磺酸盐的酯,近年来提出的方法相当强调在反应物在有机溶剂反应介质中接触之前脱水。 本发明避免了在含水条件下进行反应而使用非水溶剂的问题,但是具有可控的碱度和含水量,特别是在碱与苯酚磺酸盐摩尔比为1.3:1至1.6:1的条件下,总的水 至酚磺酸盐(作为无水物质)不超过4.5:1。 该反应优选仅使用少量摩尔过量的羧酰氯与苯酚磺酸盐相比,优选将反应温度控制在低于30℃,特别是5至20℃。在该方法的进一步改进中, 通过在反应混合物中使用小但有效量的表面活性剂,特别是醇乙氧基化物,可以改善产物中苯甲酸的增强污染。 该方法特别适用于从苯酚磺酸钠二水合物和苯甲酰氯制备苯甲酰基苯氧基苯磺酸钠。