摘要
以Ba(13)^CO_(2)为稳定同位素;C的原料,首先与硫酸(H;SO;)反应制备(13)^CO_(2),通过装有浓硫酸的干燥塔进行干燥,然后将其通过导管引入3,4-(亚甲二氧基)苯基溴化镁格氏试剂,两者反应后获得胡椒酸,再经LiAlH_(4)还原,依次加入蒸馏水,盐酸调为弱酸性,乙酸乙酯萃取有机物,除去有机相,固体用无水乙醇重结晶,得白色粉末,制得稳定同位素;C标记胡椒醇,分离收率达90%,纯度98%,其结构经核磁共振氢谱、碳谱和红外光谱鉴定。
A mild and convenient procedure for the preparation of stable(13)^C-labeled piperonyl alcohol was reported.(13)^CO_(2)was firstly prepared by means of Ba(13)^CO_(2)and sulphuric acid,then(13)^C-labeled piperic acid was prepared with(13)^CO_(2)and 3,4-(methylenedioxy)phenyl magnesium bromide,and which was reduced by LiAlH_(4),then distilled water and hydrochloric acid was adjusted to weak acidity,organic compound was extracted with ethyl acetate,the organic solution was removed,and the obtained solid was recrystallized with absolute ethanol,stable isotope(13)^C-labeled piperonyl alcohol was obtained as a white powder.The yield was 90%and the purity was 98%.Its chemistry structure was identified by;H NMR,;CNMR and IR.
作者
刘宇龙
周源彪
董凤秀
王子豪
周玥龙
周中高
Liu Yulong;Zhou Yuanbiao;Dong Fengxiu;Wang Zihao;Zhou Yuelong;Zhou Zhonggao(College of Chemistry and Chemical Engineering,Gannan Normal University,Key Laboratory of Jiangxi University for Functional Materials Chemistry,Jiangxi,341000)
出处
《当代化工研究》
2022年第7期174-176,共3页
Modern Chemical Research
基金
国家自然科学基金资助项目“糖基氮杂环卡宾过渡金属络合物及其不对称催化性能研究”(项目编号:21562002)
江西省高等学校功能材料化学重点实验室开放课题资助项目“电子传输层优化以实现高性能钙钛矿太阳能电池”(项目编号:FMC20601)
江西省教育厅基金资助项目“小尺寸手性金纳米粒子可控合成及性质研究”(项目编号:GJJ201427)
赣南师范大学大学生创新创业训练计划项目“不对称催化实现的二氧化碳固定”(项目编号:CX210052)。
