第 42 卷第 3 期Vol. 42 No. 3
2012 年 6 月Jun 2012

所属栏目:医药及中间体

5-溴代胡椒环的合成方法研究
姜 辉,赵素娟,赵 巍,王海波,王海洋*,王守凯 (中钢集团鞍山热能研究院有限公司,辽宁 鞍山 114044)
摘 要:以胡椒环为原料,采用氧化溴化体系合成5-溴代胡椒环,确定了溴化工艺条件,考察了溶剂种类、反应温度、物料配比及反应时间对反应的影响。优化工艺为:三氯甲烷为反应溶剂,反应温度为10℃,反应时间为6 h,物料配比n(胡椒环) ∶n(氢溴酸)=1∶1.2。产品收率 81%,产品纯度99.5%(GC)。产物的结构经1H NMR、IR、MS表征。
关键词:溴代胡椒环;溴化;合成
中图分类号:TQ0625.21  文献标识码:A  文章编号:1009-9212(2012)03-0047-03
Study on Synthesis of 5-Bromo-pepper Ring
JIANG Hui,ZHAO Su-juan,ZHAO Wei,WANG Hai-bo,WANG Hai-yang,WANG Shou-kai (Sinosteel Anshan Research Institute of Thermo-Energy Co.,Ltd. Anshan 114044,China)
Abstract:5-Bromo-pepper ring was synthesized from pepper ring by its bromination with H2O2/HBr or bromine. The reaction conditions of the H2O2/HBr system were investigated. The optimum conditions were as followings:chloroform as the reaction solvent,reaction temperature of 10℃,reaction time of 6 hours,molar ratio of pepper ring to hydrogen bromide of 1.0∶1.2. The target product was obtained in 81% yield(purity 99.5% GC)and its structure was confirmed with IR,1H NMR and MS.
Key words:5-bromo-pepper ring;bromination;synthesis
作者简介:姜 辉(1981-),男,辽宁鞍山人,工程师,硕士,主要从事精细化工中间体及煤焦油深加工研究。(E-mail:jianghui5168@126.com)
联 系 人:王海洋,工程师。主要从事精细化工。(E-mail:haiyangwang2008@yahoo.com.cn)
收稿日期:2012-02-13