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Liguzinediol的合成工艺优化 预览 被引量:1

Improved Synthesis of Liguzinediol
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摘要 目的确定并优化Liguzinediol的合成工艺。方法以乙酰乙酸乙酯为起始原料,经亚硝化、Pd/C催化氢化、缩合、脱氢、硼氢化钠还原得到Liguzinediol,并对各步反应条件进行优化。结果制备2-羟亚氨-3-氧代丁酸乙酯时,原料与亚硝酸钠当量比为1∶1.4,亚硝酸钠水溶液的浓度为16%最佳;制备3,6-二甲基吡嗪-2,5-二甲酸二乙酯时,反应温度30℃、1当量三乙胺、反应溶剂乙醇与原料质量比为8.8最佳;制备Liguzinediol时,反应溶剂为THF和EtOH、3当量硼氢化钠、2当量无水氯化钙、反应温度为室温最佳。产品总收率49.1%,纯度99.91%。结论此路线所用原料均廉价易得,反应条件温和,收率提高至49.1%,产品质量可控,便于放大生产。 OBJECTIVE To identify and optimize the synthesis of liguzinediol.METHODS Ethyl acetoacetate was used as the starting material to obtain liguzinediol by nitration,Pd/C catalytic hydrogenation,condensation,dehydrogenation and sodium borohydride reduction.The reaction conditions were optimized.RESULTS When ethyl N-hydroxyiminoacetoacetate was prepared,the ratio of the raw material to sodium nitrite was 1∶ 1.4,the concentration of sodium nitrite aqueous solution was16%.When diethyl 3,6-dimethyl-2,5-pyrazinedicarbonate was prepared,the reaction temperature was 30℃,1 equivalent of trimethylamine,and the mass ratio of ethanol to the raw material was 8.8.When liguzinediol was prepared,the reaction solvents were THF and EtOH,3 equivalents of sodium borohydride,2 equivalents of anhydrous calcium chloride,and the reaction temperature was room temperature.The total product yield was 49.1%,while the purity was 99.91%.CONCLUSIONThe raw materials used in this route are cheap and easy to obtain,the reaction conditions are mild,the yield is increased to 49.1%,the product quality is controllable,and it is easy to enlarge the production.
作者 蔡建国 李伟 钱程博 王天麟 何瑜芳 朱叶华 CAI Jian- guo, LI Wei , QIAN Cheng- bo, WANG Tian -lin, HE Yu -fang, ZHU Ye- hua (College of Pharmacy, Nanjing (fni'versity of Chinese Medicine, Jiangsu Key Laboratory of Therapeutic Material of Chi nese Medicine, Nanjing, 210023, China)
出处 《南京中医药大学学报》 CSCD 北大核心 2018年第3期322-324,共3页 Journal of Nanjing University of Traditional Chinese Medicine(Natural Science)
基金 国家自然科学基金(81573304) 江苏省中药资源产业化过程协同创新中心项目(ZDXM-2-1) 江苏省高校优势学科建设工程项目
关键词 乙酰乙酸乙酯 LIGUZINEDIOL 合成 工艺优化 acetoacetate liguzinediol synthesis process optimization
作者简介 蔡建国(1990-),男,硕士研究生。;通信作者:李伟,男,教授,主要从事天然产物结构修饰工作。E-mail:liwaii@126.com
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