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作 者:闫涛[1] 张在庆[1] 孙学军[1] 尤进茂[1,2]
机构地区:[1]曲阜师范大学化学与化工学院山东省生命有机分析重点实验室,山东省曲阜市273165 [2]中国科学院西北高原生物研究所,青海省西宁市810001
出 处:《曲阜师范大学学报(自然科学版)》2009年第3期61-63,共3页Journal of Qufu Normal University(Natural Science)
基 金:国家自然科学基金(20075016);山东省自然基金项目(02BS046)
摘 要:以草酸和苯甲醇为原料,采用三种不同的催化剂对甲苯磺酸、硫酸氢钾、强酸性阳离子交换树脂,三种不同的带水剂甲苯、苯、环己烷,合成了草酸二苄酯.并通过熔点、红外图谱,质谱对产物的结构进行表征.研究了反应物的配比、催化剂的种类和用量、带水剂的种类和用量对产物收率的影响.试验结果表明,当n(草酸)∶n(苯甲醇)=1∶2.2(摩尔比);催化剂为对甲苯磺酸,用量为草酸质量的0.5%(0.13 g);苯为带水剂,用量40 mL,反应时间40 min;反应产率高达96.2%.Taking oxalic acid and benzyl alcohol as raw materials, dibenzyl oxalate was synthesized by using p- toluene sulphonic acid, potassium bisultfute, strong acid ionic exchange resin as catalysts and Toluene, benzene, cyclohexane as water-carrying agents. Structure of the product was identified by means of melting point measurement, IR and LC-MS. By a single factor test, effects of the reactant ratio, variety and quantity of the catalysts and watercarrying agents on the reaction were studied. Results showed the optimal reaction conditions: were n( oxalic acid): n( benzyl alcohol) = 1:2.2 (mole ratio), p-toluene sulphonic acid 0.15 g, benzene 40 mL, reaction time 40 min,the yield of dibenzyl oxalate reached up to 96.2%.
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