有机化学 ›› 2026, Vol. 46 ›› Issue (9): 3646-3658.DOI: 10.6023/cjoc202605029 上一篇    下一篇

研究论文

酰胺还原炔基化和还原烷基化反应在Schwarzinicines A~C及Ficusnotins B, F快捷合成中的应用

陈金权, 黄培强*()   

  1. 厦门大学化学化工学院 福建省化学生物学重点实验室(厦门大学) 福建厦门 361005
  • 收稿日期:2026-05-29 修回日期:2026-07-07 发布日期:2026-07-23
  • 基金资助:
    国家自然科学基金(22571267); 国家自然科学基金(21931010)

Application of Amide Reductive Alkynylation and Reductive Alkylation in the Rapid Synthesis of Schwarzinicines A~C and Ficusnotins B, F

Jinquan Chen, Peiqiang Huang*()   

  1. Fujian Key Laboratory of Chemical Biology (Xiamen University), College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, Fujian 361005
  • Received:2026-05-29 Revised:2026-07-07 Published:2026-07-23
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    Dedicated to the 100th anniversary of the birth of Professor Xikui Jiang.

  • Supported by:
    National Natural Science Foundation of China(22571267); National Natural Science Foundation of China(21931010)

Ficusnotins B, F和Schwarzinicines A~C是近年报道的1,4-二芳基丁烷类天然产物. 尽管结构简单, 对Schwar- zinicine A初步的结构-活性研究发现了四个血管舒张活性更高和一个结构高度简化且活性相当的类似物. 报道了本课题组发展的两个酰胺转化反应在上述天然产物快捷合成中的应用. 通过仲酰胺还原烷基化反应, 即铱催化硅氢化-格氏试剂加成, 建立了Schwarzinicines A, C的两步合成法, 总产率分别为74%和75%. 通过叔酰胺还原炔基化和形式还原烷基化反应, 即铱-铜接力催化还原炔基化, 和串联钯催化氢化的“一瓶”反应, 建立了Schwarzinicine B的“两瓶”合成法, 总产率79%. 通过形式催化还原烷基化, 建立了Ficusnotins B, F的三步合成法, 总产率分别为75%和68%. 通过叔酰胺催化不对称还原炔基化反应, 即铱-铜和有机小分子接力/协同催化, 初步发展了Schwarzinicines A~C的催化不对称合成的“两瓶”法. 尽管对映选择性只有2.4∶1, 2∶1和2.4∶1, 但依据所得对映富集的产物, 可推测此前未知的Schwarzinicines A~C的绝对构型.

关键词: 天然产物, 全合成, 酰胺还原炔基化, 酰胺还原烷基化, 绝对构型

Ficusnotins B and F, along with Schwarzinicines A~C, are 1,4-diarylbutanoids reported in recent years. Despite their simple structure, preliminary structure-activity relationship studies of Schwarzinicine A analogs for vasorelaxant activity have led to the discovery of four analogs of Schwarzinicine A with significant potency improvement and a simplified analogs with a similar pharmacological profile as Schwarzinicine A. The application of two reactions previously developed by Huang’s group, reductive alkynylation and reductive alkylation of amides, in the synthesis of these five natural products is reported. A two-step synthesis of Schwarzinicines A and C was established through iridium-catalyzed hydrosilylation of secondary amides followed by in situ Grignard addition, yielding two alkaloids in overall yields of 74% and 75%, respectively. A “two-pot” synthesis of Schwarzinicine B was achieved using the iridium-copper relay-catalyzed reductive alkynylation of tertiary amide followed by tandem palladium-catalyzed hydrogenation, resulting in the formation of the alkaloid with an overall yield of 79%. By applying the latter method, a three-step synthesis of Ficusnotins B and F was developed with overall yields of 75% and 68%, respectively. Using iridium-copper and organocatalyst relay/synergistic catalysis, a two-step catalytic asymmetric syn- thesis of Schwarzinicines A~C was preliminarily developed. Although the enantioselectivities were only 2.4∶1, 2∶1, and 2.4∶1, respectively, the enantiomerically enriched products thus obtained allowed a tentative assign of the previously unknown absolute configurations of Schwarzinicines A~C.

Key words: natural products, total synthesis, reductive alkynylation of amides, reductive alkylation of amides, absolute configuration