Thioesters serve as important pharmacophores and synthetic intermediates, yet their conventional synthesis typically requires high temperatures, transition metal catalysts, or toxic and malodorous thiols. Herein, we present a simple and green electrochemical approach for the thioesterification of carboxylic acids with aromatic disulfides as direct sulfur surrogates, promoted by triphenylphosphine. The reaction proceeds under mild conditions without requiring transition metals, external reducing agents, or inert atmosphere. A broad scope of aromatic, aliphatic, and heterocyclic carboxylic acids, along with diversely substituted aromatic disulfides, are well tolerated, affording the corresponding thioesters in moderate to excellent yields. Gram‑scale synthesis and downstream derivatization demonstrate the practical utility of this protocol. Mechanistic studies support a radical–radical cross‑coupling pathway. This work offers a scalable and environmentally benign alternative for thioester synthesis.

An efficient, economical and modular route for the synthesis of fused bicyclic γ‐lactams has been achieved. Commercially accessible cyclic α‐amino acid derivatives are employed as starting materials and react with acrylates to afford fused bicyclic γ‐lactams, which are a fundamental structural motif, highly prevalent in diverse alkaloids and bioactive compounds, and a promising scaffold for developing novel antimicrobial agents against drug‐resistant microbes. The strategy sequentially proceeds through visible‐light‐induced single‐electron transfer (SET), decarboxylation, radical addition, deprotection, and cyclisation in one pot, applicable to N ‐protected and unprotected cyclic α‐amino acids, internal alkenes, as well as aromatic and aliphatic acrylates, successfully constructing diverse molecular scaffolds of fused bicyclic γ‐lactams comprising four‐, five‐, six‐, and seven‐membered rings. This protocol features broad substrate scope, mild reaction conditions, simple operation and excellent step economy.

A photocatalyzed strategy has been developed for the direct hydroacylation of diethyl benzylidenemalonates. This approach employs readily available and stable aromatic carboxylic acids as acyl radical precursors in combination with inexpensive triphenylphosphine as an efficient additive. The present system eliminates the need for complex acyl radical precursors and proceeds under mild conditions, offering a convenient and efficient route to access aromatic ketones directly from aromatic acids.

An efficient photoinduced radical-polar crossover strategy is described for the three-component carbooxygenation of arylalkenes, enabling their concomitant cyanomethylation/carbonylmethylation and esterification. This method facilitates the direct incorporation of cyanomethyl/carbonylmethyl and ester groups into readily available olefins using α-bromo nitriles/α-bromo esters and carboxylic acids as key reagents. The reaction proceeds under mild conditions at room temperature, exhibiting good functional group tolerance, a broad substrate scope, and high atom economy. Notably, despite the relatively weak nucleophilicity of carboxylic acids, they can be directly incorporated into this photoinduced radical-polar crossover transformation. Moreover, this protocol is also applicable to other nucleophiles, including alcohols, water, and aromatic amines, thereby significantly enhancing its synthetic versatility. This work offers a practical and versatile approach to constructing multifunctionalized molecules.

A photoredox-catalyzed three-component reaction has been developed, in which two distinct nitrogen-centered radicals are generated through sequential reductive and oxidative processes mediated by the photocatalyst. This transformation involves C-C bond cleavage and generation of an alpha-aminoalkyl radical as parallel key steps, enabling alkene difunctionalization to achieve N-alpha-alkylation at the alpha-C(sp3)-H site of N-aryl glycine derivatives. This method offers a novel approach for the synthesis of unnatural amino acids bearing diverse functional groups. The reaction proceeds under mild conditions and exhibits broad substrate scope, facilitating the preparation of a series of N-aryl glycine derivatives containing cyanoalkyl groups.

A visible-light photocatalytic method is reported for the regio- and stereoselective synthesis of polysubstituted γ-lactams from N-arylglycines and Morita-Baylis-Hillman (MBH) acetates. The reaction proceeds through sequential radical aminoalkylation of the dual electrophilic MBH acetate by photogenerated α-aminoalkyl radicals, forming a key γ,γ'-diaminobutyl ester intermediate that undergoes regioselective lactamization. This strategy provides a mild and efficient route to privileged γ-lactam scaffolds, demonstrating the rational integration of two versatile synthons in cascade reactions.

This work presents a novel photocatalytic halogen atom transfer (XAT) strategy, enabling redox-neutral C(sp3)-C(sp3) coupling between N-aryl tetrahydroisoquinolines and unactivated alkyl halides. The strategy employs an α-aminoalkyl radical, generated in situ from N-aryl tetrahydroisoquinoline via single-electron transfer (SET) oxidation under photocatalytic conditions. This radical acts as a traceless XAT reagent to activate alkyl bromides/chlorides/iodides (C-X bond), forming key alkyl carbon radicals. Simultaneously, the same N-aryl tetrahydroisoquinoline molecule is converted into an iminium intermediate after the XAT event, which functions as an endogenous coupling partner to capture the alkyl radicals, ultimately forming C-C bonds. This transformation proceeds under redox-neutral conditions without external XAT reagents or stoichiometric reductants.

In this work, we present a novel electrochemical strategy for the direct conversion of methylarenes to aromatic nitriles, employing hydroxylamine sulfate as a safe, green, and economical nitrogen source. This transformation proceeds in an undivided cell without the need for transition-metal catalysts, chemical oxidants, or dehydrating agents, enabling efficient conversion of inert methylarenes into valuable aromatic nitrile compounds. Notably, this approach effectively circumvents the use of highly toxic cyanating reagents typically required in conventional nitrile synthesis. The practicality and potential application value of this methodology are demonstrated through gram-scale reactions and diverse derivatization of the cyano group. This electrochemical protocol not only provides a new strategy for constructing aryl nitriles but also expands the synthetic scope of electrochemical C-H functionalization.

An environmentally benign electrochemical reductive method has been developed for the hydroselenization/hydrosulfuration of vinyl sulfones with diselenides/disulfides. The reaction proceeds smoothly in an undivided cell at room temperature in open air, without the need for metal catalysts or oxidants, achieving yields of up to 99% for 37 β‐selenosulfones and β‐thiosulfones. This strategy is also applicable to other electron‐deficient olefins, providing a mild and efficient approach for constructing C─Se and C─S bonds.

The dihydroquinolin-2-one scaffold is a privileged structure in many bioactive compounds. We describe a visible-light-driven photoredox catalysis strategy for the decarboxylative coupling of 2-quinolinones with α-amino acids, enabling the efficient synthesis of 3-aminoalkyl dihydroquinolin-2-ones. This method utilizes readily available α-amino acids to generate α-aminoalkyl radicals under mild conditions. It exhibits a broad substrate scope, accommodating natural α-amino acids (both cyclic and acyclic), other α-heteroatom-substituted acids, and aliphatic carboxylic acids. This redox-neutral transformation proceeds under simple conditions with good functional group tolerance, eliminates the need for sacrificial reagents or hydrogen atom donors, and exhibits good step economy. Decarboxylation generates CO2 as the only byproduct.

A novel and environmentally benign electrochemical method has been developed for the regioselective C6 thiocyanation of tetrahydroquinolines using potassium thiocyanate (KSCN) as an inexpensive and readily available thiocyano source. This transition-metal-free and oxidant-free protocol proceeds under mild conditions, enabling efficient construction of C(sp²)-SCN bonds. Utilizing TEMPO as a redox mediator, the reaction affords 6-thiocyanato-tetrahydroquinoline derivatives in moderate to good yields. The protocol is also applicable to the C4 thiocyanation of anilines and the C6 selenocyanation of tetrahydroquinolines. The method demonstrates excellent regioselectivity, high atom economy, broad substrate scope, and good functional group compatibility, providing a practical approach to a range of valuable thiocyanated and selenocyanated derivatives. An environmentally benign electro-chemical method for the regioselective C6 thio-/selenocyantion of tetrahydroquinolines.

A novel electrochemical method for the direct synthesis of 2-thiazolidinone derivatives is reported. Readily available aryl alkenes, KSCN and H2O are utilized as starting materials to produce 4-aryl-2-thiazolidinones in moderate to satisfactory yields. KSCN acts as a radical precursor and nucleophile, while H2O participates in the formation of carbamoyl groups, ensuring high atom economy. The reaction proceeds under mild and environmentally friendly conditions, constructing the 2-thiazolidinone heterocycle without the need for metals, catalysts, external oxidants, or sacrificial agents. It exhibits excellent product diversity and functional-group tolerance. The reaction is conducted in an undivided cell under open-air conditions and is operationally simple. Late-stage modification of natural products, and scale-up synthesis further demonstrate the practical application of the method.

This paper describes a visible-light-mediated three-component dicarbofunctionalization of alkenes via a tandem radical addition reaction of two different alkenes triggered by aminoalkyl radicals derived from N-phenyl glycines. This method allows for one-pot skeletal assembly, providing efficient and straightforward access to structurally complex gamma-amino sulfone derivatives directly from readily available and simple starting materials. Beyond the convenience of the one-pot protocol, this method also demonstrates broad substrate scope, excellent functional group compatibility, mild reaction conditions, and ease of scalability.

A visible-light-mediated strategy is reported for the direct synthesis of polychlorinated vicinal diaryl alkanes from aryl alkenes and chloroform. In this approach, two haloalkyl radicals generated from chloroform via halogen atom transfer (XAT) and direct single electron transfer (SET) within the same photoredox catalysis cycle enable the 1,4-dichloromethyldimerization of alkenes. Besides chloroform, this strategy is applicable to carbon tetrachloride, bromotrichloromethane, and α-bromo carboxylic esters, yielding corresponding 1,4-disubstituted vicinal diaryl alkanes. Diverse polychlorinated structures containing highly congested vicinal quaternary carbon centers are effectively synthesized by this method. The potential of this reaction in late-stage drug modification is highlighted by the successful transformation of olefins with pharmaceutical structures.

A novel visible-light-induced cascade cyclization strategy for the synthesis of 4H-3,1-benzoxazines from benzoquinone and alkynylanilides is described. This transition metal- and oxidant-free method utilizes direct photoexcitation of benzoquinone to its triplet state, eliminating the need for additional photosensitizers. The process generates tetrasubstituted carbon-centered 4H-3,1-benzoxazine compounds bearing both acyl and phenolic substituents. The method exhibits broad substrate compatibility, high atom economy, and operational simplicity, providing an environmentally benign route to diverse 4H-3,1-benzoxazine derivatives-privileged scaffolds in medicinal chemistry.

This article presents a method for asymmetric formal cross-dehydrogenative coupling of benzylic alcohols with ketones through combined electrooxidation and organocatalysis. Employing inexpensive and environmentally friendly proline as a chiral organocatalyst, various benzylic alcohols and simple ketones serve as substrates to directly obtain diverse chiral beta-hydroxycarbonyl compounds with moderate to good yields (up to 85%) and excellent stereoselectivity (up to 99% ee and 99:1 dr). The reaction proceeds under mild conditions at room temperature in air, without oxidants or additives, demonstrating robust functional group tolerance and atom efficiency. Hydrogen gas released at the cathode is the sole byproduct. Using L- or D-proline allows straightforward access to both chiral configurations of beta-hydroxycarbonyl compounds.

Herein, an electrochemical tandem reaction that integrates acetonitrile self‐coupling with selenylation to construct densely functionalized tetrasubstituted alkenes bearing amino, cyano, and seleno groups from readily available acetonitrile and diselenides is reported. Employing potassium iodide as a redox mediator under mild, metal‐free, and oxidant‐free conditions, this sustainable strategy leverages the synergistic effect of electrochemical oxidation and iodine catalysis to achieve inert C(sp3)H bond activation of acetonitrile. The transformation exhibits good stereoselectivity along with substrate scope across diverse aryl and alkyl selenides.

This article reports the first example of multi‐component hydroxy‐thiocarbamation of electron‐deficient alkenes in an electrochemical undivided cell. Simple and readily available electron‐deficient (hetero)aryl alkenes, KSCN and H 2 O are used as starting materials to produce β‐hydroxy primary S‐thiocarbamate derivatives in moderate to good yields. H 2 O is involved in the formation of carbamoyl and hydroxyl groups, making the method highly atom‐economical. The reaction introduces multiple functional groups under mild and environmentally friendly conditions, without the need for metals or external oxidants. The reaction exhibits good functional‐group tolerance and excellent product diversity. The procedure is operationally simple, and late‐stage modification of natural products further demonstrates the practical application of the method.

An electrochemical method for selenylating tetrahydroquinolines with diselenides is presented. By tuning reaction conditions, C-3 selenylated quinolines and C-6 selenylated tetrahydroquinolines can be selectively synthesized with excellent outcomes.

A visible-light-induced decarbonylation/Truce-Smiles rearrangement cascade has been developed for the direct synthesis of 2-aminobenzophenones. This protocol employs readily available isatins and sulfonyl chlorides as starting materials, enabling the construction of diverse 2-aminobenzophenone derivatives under mild conditions without the need for transition metal catalysts or photocatalysts. The reaction exhibits a broad substrate scope, excellent functional group tolerance, and high efficiency. A total of 32 derivatives were synthesized with yields that reached 99%. The practicality of this approach was further demonstrated through a gram-scale reaction, highlighting its potential for synthetic applications.