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机构地区:[1]渤海大学化学化工学院,锦州121000 [2]渤海大学科技实验中心,锦州121000 [3]辽宁石油化工大学石油化工学院,抚顺113001
出 处:《香料香精化妆品》2007年第5期11-13,共3页Flavour Fragrance Cosmetics
摘 要:以对叔丁基苯甲酸和甲醇为原料,甲基磺酸为催化剂合成对叔丁基苯甲酸甲酯,考察两种不同生产工艺A、B。工艺A采用一步法,当酸醇摩尔比1∶7,催化剂10%(占酸的摩尔份数),回流反应8h时,产率为85.8%。在上述条件下,工艺B将反应分两个阶段进行,第一阶段酸醇摩尔比1∶3.5,回流反应3h后蒸除水和甲醇;再加入与第一阶段同样量的甲醇,继续回流反应5h,产率高达95.3%。产品经红外和折光率进行表征。p-tert-Butyl benzoic acid methyl ester was synthesized from p-tert-butyl benzoic acid and methanol using methanesul fonic acid as catalyst by two different production processes A and B. Process A used the one-step method, the yield 85.8% was obtained when the molar ratio of acid to alcohol is 1 : 7, 10% catalyst (molar percent of acid), and refluxed for 8 h. Under the same condition, the reaction was performed using process B, which was separated for two stages. In the first stage, the molar ratio of acid to methanol is 1 : 3.5, methanol and the produced water were separated by distillation after refluxed for 3 h. Then the same amount of methanol as the first stage was added, the reaction refluxed for further 5 h, the yield of product was up to 95.3 %. The product was characterized by 1R and index of refraction.
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