己酸正丁酯的绿色合成.pdf

中国食品添加剂
China Food Additive
试验研究
已酸正丁脂的绿色合成
马翠丽1,李玉文2,
1.青岛农业人学校医院,青岛266109;2.青岛衣业人学化学与药学院,青岛266109
摘要:采川己酸和倗酸丁帝为原料,在死催化剂、元溶剂条件下加热反应合成葡笱酒香料己酸正丁
当,测定所合成的葡萄滷香料己酸正∫脂的红外光谱及折射率并与文献报道值相比较,从而确证所合成的己俊
正丁的结构。考察了反应温度、反应物配比、反应时间等对己酸正丁收率的影响。确定了最佳反应条件
(硼酸三J啃):n(已酸)=3:1,反应温度110℃,反应时间8l,在此条件下化率达97.8%,所得己酸
正丁产品的纯度达到995%。此外,该方法收率高,易于纯化,所得副产物酸可川于制各硼酸三丁席,
量的硼梭三」脂原料以回收循坏使用,整个过程无三废排放,绿色坏保,具有⊥业化前景。
关键词:酸正丁;硼酸二丁;山酸;绿色合成
中图分类号:IS202.3
文献标识码:A
文章编号:1006-2513(2015)10-0062-03
Green synthesis of n-butyl hexanoate
MACu-li,IIYu-wcn2,°
(1. School Hospilal, Qingdao Agricultural University, Qingdao 266109; 2. School of Pharmacy and
Chemistry, Qingdao Agricultural University, Qingdao 266109
Abstract: Rcaction of hexanoic acid with tributyl borale in the absence of solvent and calalyst gavc rise to n butyl
hexanoate. The structure of n-butyl hexanoate was confirmed by measuring and comparing melting point and TR
with that reported in literature. The eflects o! reaction temperalure, mole ralio o! reactants and reaction time on the
esterification rate were investigated. The most suitable reaction conditions were determined as follows: the mole ratio
of tributyl borate to hexanoic acid was 3: 1, the reaction temperature was 110C, and reaction time was 8 h. And the
esterification rate of hexanoic acid can reach.%under this reaction condition, and the purity of n-butyl hexanoate
was up to 99. 5%. Moreover, this green synthetic procedure has the advantage o! high yield and easy purification, th
by-products can be used for preparation of tributyl borate, the excessive tributyl borate can be recycled, the whole
process has no three-waste discharge and is green, which also has a industrialization prospect
Key words: n-butyl hexanoate; tributyl borate; hexanoic acid; green synthesis
作为食用?料,己酸正丁酯主要用于配制葡
基于上述研究已酸正酯否料的合成具有
萄漕等?,能提高萄漕的品质,从而増强销重要意义。当前,已酸正丁帖生产一般采已酸和
芍酒的市场完争力。人们生活水平的提高促进正.J醇为原料,在各种不同酸性催化剂作用下
了对匍萄滷的消费,使爪香料的需求也日益增合成,所用催化剂主要包括:浓硫酸、固体酸
等。浓硫酸催化导致副反应,从而产品收率
收稿日期:2015-06-09
基金项目:国家白然科学基金(N。.2107211),l东省自然科学基金(No.ZR201BL003),青岛农业大学博士基金(N。.630708)。
作者筒介:李土文(1969),男,山东芭县人,副教授,博上,研究方向为药物化学。
通信作者:李三文,L-mail: ywli(Qqau edu.cn。
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