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Esterification of salicylic acid with methanol/dimethyl carbonate over anion-modified metal oxides

机译:在阴离子改性的金属氧化物上用甲醇/碳酸二甲酯酯化水杨酸

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摘要

The esterification of salicylic acid to methyl salicylate over solid acids such as zirconia,alumina and silica and their sulphate,phosphate and borate modified forms,has been studied for the first time in an autoclave under autogenous conditions using methanol and dimethyl carbonate to compare their methylating ability.Metal oxides such as zirconia,alumina and silica as well as their sulphate,phosphate and borate modified forms are effective catalysts for the conversion of salicylic acid to methyl salicylate.Superacid,sulphated zirconia,is the most suitable catalyst due to high yield,selectivity,reusability and the simple method used for the preparation of the catalyst.The percentage yield of methyl salicylate was found to be higher when methanol was used as the methylating agent over these catalysts rather than dimethyl carbonate.Hence,methanol appears to be a better methylating agent compared to dimethyl carbonate in terms of yield as well as atom economy.The influence of reaction temperature,amount of catalyst,duration of reaction and molar ratio of salicylic acid:methanol/dimethyl carbonate has been studied over sulphated zirconia.
机译:水杨酸在固体酸如氧化锆,氧化铝和二氧化硅及其硫酸盐,磷酸盐和硼酸盐改性形式上被水杨酸酯化成水杨酸甲酯,这是首次在高压釜中在自生条件下使用甲醇和碳酸二甲酯比较它们的甲基化金属氧化物如氧化锆,氧化铝和二氧化硅及其硫酸盐,磷酸盐和硼酸盐的改性形式是将水杨酸转化为水杨酸甲酯的有效催化剂。由于高收率,硫酸,硫酸化的氧化锆是最合适的催化剂,选择性,可重复使用性和制备催化剂的简单方法。当甲醇用作甲基化剂而不是碳酸二甲酯时,水杨酸甲酯的百分收率更高。因此,甲醇似乎更好甲基化剂与碳酸二甲酯相比,在收率和原子经济性方面都很好。研究了硫酸化氧化锆的性能,催化剂用量,反应时间和水杨酸:甲醇/碳酸二甲酯的摩尔比。

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