贝诺酯合成工艺优化  

Optimization of Benorilate Synthesis Process

作　　者：赵莉娜 刘方蕊 李曼 王智贤 曹江营 Zhao Lina;Liu Fangrui;Li Man;Wang Zhixian;Cao Jiangying(School of Pharmacology,Shandong University of Traditional Chinese Medicine,Jinan 250355,China)

机构地区：[1]山东中医药大学药学院,山东济南250355

出　　处：《山东化工》2024年第14期33-37,共5页Shandong Chemical Industry

基　　金：山东省医药卫生科技发展计划项目(202013051070);山东中医药大学大学生创新训练计划项目(2023055)。

摘　　要：以乙酰水杨酸为原料,氯化亚砜为氯代试剂,吡啶为催化剂,制得乙酰水杨酰氯。四氢呋喃为溶解乙酰水杨酰氯溶剂,TBAB为相转移催化剂,在5%氢氧化钠碱性条件下,对乙酰氨基酚与乙酰水杨酰氯缩合60 min,得到贝诺酯。对乙酰氨基酚和乙酰水杨酸的物质的量之比为1∶1.2。此工艺路线温和,后处理和纯化简单。总收率为69%。所得产物经过1H-NMR和13 C-NMR确证结构。Using pyridine as the catalyst and sulfoxide chloride as the chlorinated reagent,acetylsalicylic acid underwent substitution reaction to give acetylsalicyloyl chloride.Then,using tetrahydrofuran as the solvent to dissolve the acetylsalicyloyl chloride and TBAB as the phase transfer catalyst,acetaminophen was condensed with acetylsalicyloyl chloride for 60 minutes to give benorilate under the alkaline condition of 5%sodium hydroxide.The mole ratio of acetaminophen to acetylsalicylic acid is 1∶1.2.The synthesis process is mild,with simple post-treatment and purification.The total yield is 69%.The target product was structurally confirmed by 1H-NMR and 13 C-NMR.

关 键 词：贝诺酯 合成 优化 相转移催化剂 

分 类 号：TQ460[化学工程—制药化工]