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目的改进天然产物黄连碱的合成工艺。方法以2,3-二羟基苯甲醛为起始原料,经环合、缩合和闭环3步反应得到目标化合物黄连碱。其中,主要针对第二步缩合反应的纯化步骤以及第三步闭环反应的溶剂选择和纯化过程做了有效的改进工作。结果中间体和目标产物结构经1H-NMR、13C-NMR图谱数据确证,总收率可达43.0%,目标化合物经HPLC检测纯度高达98.5%。结论改进后的合成方法反应步骤少、操作简单、条件温和、产物收率及纯度较高,有利于工业化生产。
Objective To improve the synthetic process of natural product Coptis alkali. Methods Starting from 2,3-dihydroxybenzaldehyde, the target compound coptisine was obtained via cyclization, condensation and ring closure in 3 steps. Among them, the purification process of the second condensation reaction and the solvent selection and purification process of the third-stage closed-loop reaction are mainly improved. Results The structures of intermediates and target compounds were confirmed by 1H-NMR and 13C-NMR. The total yield of the intermediates and target compounds was 43.0%. The purity of the target compounds was 98.5% by HPLC. Conclusion The improved synthesis method has fewer reaction steps, simple operation, mild conditions and high product yield and purity, which is beneficial to industrialized production.