合成水杨酸甲酯的实验条件探究_竹李帅.pdfVIP

化 学 工 程 师 Sum213No.6 Chemical Engineer 2013年第6期 文章编号：1002-1124 （2013）06-0012-03 科 研 与 合成水杨酸甲酯的实验条件探 究 * 开 发 竹李帅 1a ，熊双喜 1b ，龙 威 2* （1.台州学院 a.生命科学学院；b.医药化工学院，浙江台州317000；2.南华大学化学化工学院，湖南 衡阳 421001） 摘 要：甲醇和水杨酸合成水杨酸甲酯是药物化学合成的热点。在NaHSO·HO作为主要催化剂的前提 4 2 下,通过实验研究了催化剂、甲醇用量与反应时间的关系，着重分析了带水剂因素对合成水杨酸甲酯收率的影 响。实验结果表明：甲醇 ∶水扬酸摩尔比为0.60∶0.10、NaHSO·HO质量为0.30g、HSO质量为0.80g、带水 4 2 2 4 剂体积为4.00mL时，回流分水时间为3.0~3.5h为水杨酸酯甲酯的最佳实验条件，最高产率约为77.0%。 关键词：水杨酸甲酯；复合催化剂；药物化学合成 中图分类号：O641;TQ245.1文献标志码：A Experimental conditions investigation about synthesis of methylis salicylas* ZHU Li-shuai1a，XIONG Shuang-xi1b，LONG Wei2* （1.a.Department of Life Science;b.Department of Pharmaceutical and Chemical Engineering, Taizhou College, Taizhou 317000, China; 2. School of Chemistry and Chemical Engineering, University of South China, Hengyang 421001, China） Abstract ：Methanol and salicylic acid is a hot drug chemical synthesis in high yield synthesis methylis salicy － las. In this paper, it studies dosage of sodium bisulfate catalyst, methanol dosage and response time, with admixture of select catalytic synthesis of methyl salicylate and other factors on the yield effects under conditions of water combined with sodium bisulfate catalyst, methanol and salicylic acid by high-yield synthesis of methyl salicylate. Experimental results demonstrate that Ester yields was upto 77.0% for the best conditions, when methanol: water acid mole ratio of 0.6∶0.1 and sodium bisulfate is 0.3g, sulfuric acid in water 0.80g, 4mL returni