文献类型：期刊文献

中文题名：抗氧剂168的连续流高效制备

英文题名：Highly Efficient Synthesis of Antioxidant 168 in Continuous Flow

作者：茅梦梅[1,2];万力[1,2];辛忠[1,2]

机构：[1]华东理工大学上海市多相结构材料化学工程重点实验室,上海200237;[2]华东理工大学化工学院化学工程联合国家重点实验室,上海200237

年份：2019

卷号：36

期号：10

起止页码：2151

中文期刊名：精细化工

外文期刊名：Fine Chemicals

收录：CSTPCD;;EI(收录号：20194807740987);Scopus;北大核心:【北大核心2017】；CSCD:【CSCD2019_2020】；

基金：国家自然科学基金(21776080);中央高校基本科研业务费专项资金(50321011918010,50321011917025)

语种：中文

中文关键词：抗氧剂168;2,4-二叔丁基苯酚;三氯化磷;连续流动;精细化工中间体

外文关键词：antioxidant 168;2,4-di-tert-butylphenol;phosphorus trichloride;continuous flow;fine chemical intermediates

摘要：以2,4-二叔丁基苯酚和三氯化磷为原料,通过酯化反应连续流合成抗氧剂168,考察了反应溶剂、缚酸剂种类及用量、反应温度、反应停留时间对抗氧剂168收率的影响,并通过熔点、GC、1HNMR、13CNMR和HRMS对合成产物进行了表征。结果表明,最佳工艺条件为:n(2,4-二叔丁基苯酚)∶n(三氯化磷)∶n(三乙胺)=3.0∶1.0∶3.3,甲苯为溶剂,反应温度为75℃,反应停留时间为240 s,经后处理,精制产物收率可达90%,气相色谱纯度大于99.9%。
A novel method for the synthesis of antioxidant 168 was developed in continuous flow by esterification of 2,4-di-tert-butylphenol and phosphorus trichloride.The effects of reaction solvent,acid-binding agent types and dosage,reaction temperature and reaction residence time on the yield of antioxidant 168 were investigated.The target product was characterized by melting point,GC,1HNMR,13CNMR and HRMS.The results showed the optimum conditions were determined as follows:n(2,4-ditertbutylphenol)∶n(phosphorus trichloride)∶n(triethylamine)=3.0∶1.0∶3.3,toluene as solvent,reaction temperature 75℃,reaction residence time 240 s.The yield of refined product was 90%under the optimum conditions,and the purity exceeded 99.9%.