第 42 卷第 2 期Vol. 42 No. 2
2012 年 4 月Apr 2012

所属栏目:香精香料

N,N-二乙基-3,7-二甲基-(Z)-2,6-辛二烯-1-胺的合成研究
杨 阳1,尤亚华1*,姚日生2,3 (1. 合肥工业大学 化学工程学院,安徽 合肥 230009;2. 合肥工业大学 医学工程学院,安徽 合肥 230009;3. 农产品生物化工教育部重点实验室 生物化工与制药工程研究所,合肥 安徽 230009)
摘 要:以异戊二烯(IP)和二乙胺(DEA)为原料,在正丁基锂催化下合成了N,N-二乙基-3,7-二甲基-(Z)-2,6-辛二烯-1-胺(NDEA)。利用气谱分析NDEA,考察了不同因素对合成NDEA的影响,确定了较优的工艺条件:原料配比n(IP)∶n(DEA)= 4.5∶1.0,n(n-BuLi)∶n(IP)=2∶3,反应温度为环己烷的回流温度,反应时间为13 h。产品收率>55%(n/n),经减压分馏后产品纯度>97%。
关键词:合成香料;异戊二烯;N,N-二乙基-3,7-二甲基-(Z)-2,6-辛二烯-1-胺
中图分类号:O629.9  文献标识码:A  文章编号:1009-9212(2012)02-0041-03
A Study on Synthesis of N,N-Diethyl-3,7-dimethyl-(Z)-octadien-1-amine
YANG Yang1,YOU Ya-hua1*,YAO Ri-sheng2,3 (1. School of Chemical Engineering,Hefei University of Technology,Hefei 230009,China;2. School of Medical Engineering,Hefei University of Technology,Hefei 230009,China;3. Engineering Research Center of Bioprocess of Ministry of Education,Hefei 230009,China)
Abstract:N,N-Diethylnerylamine(NDEA),an important intermediate for organic synthesis,was prepared from isoprene and diethylamine catalyzed by n-BuLi in cyclohexane. The mechanism of the reaction was discussed,and NDEA was analyzed with GC. The effects of different factors on the reaction were studied. The optimum reaction conditions were as follows:the molar ratio of IP to DEA 4.5 to 1,of IP to n-BuLi 2∶3,reaction time 13 h,in refluxed cyclohexane. NDEA was resulted in 55% yield with a purity of 97% after fractional distillation.
Key words:synthetic perfume;isoprene;N,N-diethylnerylamine
基金项目:合肥市科技攻关项目(2010HKKJ0237)。
作者简介:杨 阳(1987-),男,安徽合肥人,硕士研究生,研究方向:精细化学品与绿色化学。(E-mail:yangyang870521@sina.com)
联 系 人: 尤亚华,副教授,硕士。研究方向:工业分析与精细有机化工。(E-mail:rishengyao@163.com)
收稿日期: 2012-04-0