化学学报 上一篇    

研究论文

可见光驱动的 N-芳基丙烯酰胺与芳基卤化物环化/芳基化反应

雷平, 马传超, 阿布拉江·克依木*   

  1. 新疆大学 化学学院 碳基能源化学与利用国家重点实验室 乌鲁木齐 830017
  • 投稿日期:2026-08-28
  • 基金资助:
    感谢新疆一流科技领军人才项目(XJRC-2025-KJ-PY-KJLJ-043)、上海合作组织科技伙伴计划(2022E01049)和国家自然科学基金(21961038)的资助.

Visible-light-driven cyclization/arylation of N-arylacrylamides with aryl halides

Lei Ping, Ma Chuanchao, Keyume Ablajan*   

  1. State Key Laboratory of Chemistry and Utilization of Carbon Based Energy Resources, College of Chemistry, Xinjiang University, Urumqi, 830017, PR China
  • Received:2026-08-28
  • Contact: *E-mail: ablajan209@hotmail.com, ablajan209@xju.edu.cn; Tel.: +86-13999135640
  • Supported by:
    Project supported by Technology Innovation Leading Talent Project of Xinjiang (XJRC-2025-KJ-PY-KJLJ-043), the Shanghai Cooperation Organization Science and Technology Partnership Program (N2022E01049), and the National Natural Science Foundation of China (21961038).

本文报道了一种在可见光驱动下、无需金属催化剂和光催化剂合成 3,3-二取代吲哚-2-酮的方法. 底物直接受光激发,引发 C-X 键均裂,形成芳基自由基,进而实现 N-芳基丙烯酰胺的分子内芳基化环化反应. 该方法操作简便、无需添加剂,具有优良的官能团兼容性和较高的反应效率,并可实现克级规模制备,为吲哚-2-酮骨架的可持续合成提供了一条新途径.

关键词: 可见光诱导反应, 吲哚-2-酮, 芳基卤化物, N-芳基丙烯酰胺, 无催化剂合成

Oxindoles constitute privileged heterocyclic scaffolds frequently encountered in natural products, pharmaceuticals, and other biologically active compounds. Herein, we disclose an operationally simple, visible-light-driven arylative cyclization of N-arylacrylamides with aryl halides, providing rapid access to structurally diverse 3,3-disubstituted oxindoles without transition metals or exogenous photocatalysts. Under the optimized conditions, an N-arylacrylamide, an aryl halide, and diisopropylethylamine (DIPEA) are dissolved in dimethyl sulfoxide and irradiated with 18 W violet light-emitting diodes at room temperature for 20 h. Unlike established approaches that rely on metal catalysts, photocatalysts, or additional activating reagents, this protocol uses readily available aryl halides as aryl radical precursors and proceeds under additive-free conditions. The method accommodates a range of substituents on the N-aryl moiety and the aryl halide coupling partner, demonstrating good functional-group tolerance and enabling the preparation of various oxindole derivatives. The method's synthetic practicality is further supported by successful gram-scale synthesis. Control experiments establish that both light and DIPEA are indispensable for productive conversion. The reaction proceeds efficiently under nitrogen but is almost completely suppressed by oxygen. Furthermore, addition of 2,2,6,6-tetramethylpiperidin-1-oxyl inhibits cyclization, indicating the involvement of radical intermediates. Light on/off experiments reveal that product formation occurs only during irradiation and ceases in the dark, confirming the essential role of continuous illumination. Based on these observations, we propose a plausible pathway involving photoinduced activation of the carbon-halogen bond and formation of an aryl radical. Regioselective radical addition to the acrylamide, followed by intramolecular cyclization, oxidation, and deprotonation, furnishes the desired oxindole. Overall, this catalyst-free transformation combines mild conditions, broad substrate compatibility, scalability, and reduced reagent requirements, thus providing a practical and sustainable route to valuable oxindole scaffolds. Nevertheless, the limited reactivity of less activated coupling partners remains to be addressed.

Key words: Visible-light-induced reaction, Oxindoles, Aryl halides, N-Arylacrylamides, Catalyst-free synthesis