| 蔡建国，李伟*，钱程博，王天麟，何瑜芳，朱叶华.Liguzinediol的合成工艺优化[J].南京中医药大学学报(社会科学版),2018,34(3):322-326. |
| Liguzinediol的合成工艺优化 |
| Improved Synthesis of Liguzinediol |
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| DOI： |
| 中文关键词: 乙酰乙酸乙酯 Liguzinediol 合成 工艺优化 |
| 英文关键词: acetoacetate liguzinediol synthesis process optimization |
| 基金项目: |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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 was 16%. 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%. CONCLUSION The 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. |
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