5-溴代胡椒环的合成方法研究

Study on Synthesis of 5-Bromo-pepper Ring

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。

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.