3,5-二氯苯甲醇的合成工艺改进  

Process Improvement for Synthesis of 3,5-dichlorobenzyl alcohol

作　　者：刘诗雨 寇玉辉 梅期红 李宗森 杨俊 LIU Shiyu;KOU Yuhui;MEI Qihong;LI Zongsen;YANG Jun(Guangdong Yinzhu Pharmaceutical Technology Co.,Foshan 528315,China;Guanzhou Yinzhu Biomedical Technology Co.,ltd,Guangzhou 510700,China)

机构地区：[1]广东银珠医药科技有限公司,广东佛山528315 [2]广州银珠生物医药科技有限公司,广东广州510700

出　　处：《合成化学》2023年第5期389-393,共5页Chinese Journal of Synthetic Chemistry

基　　金：广东省科技专项资金(2019FSDZX01010301)。

摘　　要：3,5-二氯苯甲醇是一种重要的医药化工原料,是多种药物的合成片段。本文以3,5-二氯苯甲酰氯为原料,硼氢化钾为还原剂,氯化锌为催化剂合成3,5-二氯苯甲醇,考察了还原剂用量、催化剂用量、溶剂用量、反应温度和溶剂套用等因素对反应的影响。实验结果表明:在3,5-二氯苯甲酰氯与硼氢化钾和氯化锌的物质的量之比为1.0∶0.9∶0.1,THF总体积为6.5 vol,反应温度为回流时,平均收率达到88.9%,反应结束后溶剂可常压蒸馏回收套用。与现有方法相比,该工艺大幅降低了硼氢化钾和氯化锌的用量,并提高了反应安全性。具有成本低和收率高的特点。3,5-Dichlorophenyl methanol is an important material in pharmacy and chemical industries,which has been used as building block for many drugs.In this work,3,5-dichlorophenyl methanol was prepared from 3,5-dichlorobenzoyl chloride using KBH 4 as the reductant,and ZnCl 2 as the catalyst.The effects of the amounts of reductants,catalysts,and solvents,as well as the reaction temperature and the use of recovered solvents were systematically evaluated.The experimental results indicated that the average yield of the reaction can reach 88.9%using 1.0∶0.9∶0.1 mol ratio of 3,5-dichlorobenzoyl chloride,KBH 4 and ZnCl 2,6.5 equivalents(vol)of THF under refluxing.In addition,the solvent can be recycled and reused,which has little effect on the efficiency of the reaction.Compared with the existing protocols,this optimal process reduced the amounts of KBH 4 and ZnCl 2 dramatically meanwhile increased the safety,which also features low cost and high yield.

关 键 词：3 5-二氯苯甲醇 3 5-二氯苯甲酰氯 硼氢化钾 氯化锌 工艺改进 

分 类 号：TQ[化学工程]