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Here, we investigate how electrolyte composition, and specifically halide identity, governs the selective electrochemical hydrogenation of acetophenone to 1-phenylethanol on copper electrodes under near-neutral aqueous conditions. Potassium halide electrolytes introduce specific halide-surface interactions that modulate hydrogen adsorption, delay HER onset, and influence organic reduction behavior. Among the halides studied, chloride- and bromide-containing electrolytes exhibit higher activity and selectivity toward 1-phenylethanol formation than iodide, highlighting a strong dependence of catalytic performance on halide identity. Systematic variation of applied potential, electrolyte identity, halide composition, and acetophenone concentration reveal strong correlations between catalytic performance and electrolyte-dependent interfacial chemistry. Kinetic analysis, hydrogen scavenging experiments, and electrochemical in situ surface-enhanced Raman spectroscopy suggest a surface-mediated hydrogenation pathway involving adsorbed acetophenone and surface-derived hydrogen species, consistent with a Langmuir\u2013Hinshelwood-like mechanism. Density functional theory calculations of hydrogen and halide coadsorption on Cu(111) provide molecular-level insights into these observations, showing that iodide remains more stable on the copper surface at cathodic potentials than chloride or bromide. This persistent iodide coverage limits surface accessibility for acetophenone adsorption, resulting in reduced hydrogenation activity despite delayed HER. Together, these results demonstrate how halide electrolyte identity tunes surface coverage, reaction kinetics, and selectivity during electrochemical hydrogenation, highlighting electrolyte engineering as an effective strategy for enabling selective ketone reduction under mild, near-neutral conditions.<\/jats:p>","DOI":"10.1021\/jacsau.6c00452","type":"journal-article","created":{"date-parts":[[2026,6,23]],"date-time":"2026-06-23T18:05:17Z","timestamp":1782237917000},"page":"3889-3902","source":"Crossref","is-referenced-by-count":0,"title":["Halide Electrolyte\nEffects in the Electrochemical\nHydrogenation of Ketones on Copper"],"prefix":"10.1021","volume":"6","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3513-7069","authenticated-orcid":true,"given":"Jose","family":"Solera-Rojas","sequence":"first","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Didac A.","family":"Fenoll","sequence":"additional","affiliation":[{"name":"Center for Cooperative Research on Alternative Energy (CIC energiGUNE), Basque Research and Technology Alliance (BRTA) , ,","place":["Vitoria-Gasteiz, Spain, 01510"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Elena","family":"Segura-Sanchis","sequence":"additional","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"M. Consuelo","family":"Barrantes","sequence":"additional","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0004-9563-4117","authenticated-orcid":true,"given":"Conor","family":"Brennan-Pollak","sequence":"additional","affiliation":[{"name":"Trinity College Dublin , , College Green , , ,","place":["Dublin 2, Dublin, Ireland"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7503-1245","authenticated-orcid":true,"given":"Francisco","family":"Fabregat-Santiago","sequence":"additional","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4432-5697","authenticated-orcid":true,"given":"Carmen","family":"Mejuto","sequence":"additional","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1348-4692","authenticated-orcid":true,"given":"Max","family":"Garci\u0301a-Melchor","sequence":"additional","affiliation":[{"name":"Center for Cooperative Research on Alternative Energy (CIC energiGUNE), Basque Research and Technology Alliance (BRTA) , ,","place":["Vitoria-Gasteiz, Spain, 01510"]},{"name":"Trinity College Dublin , , College Green , , ,","place":["Dublin 2, Dublin, Ireland"]},{"name":"IKERBASQUE, Basque Foundation for Science , Plaza de Euskadi 5 , ,","place":["Bilbao, Spain, 48009"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2308-0635","authenticated-orcid":true,"given":"Elena","family":"Mas-Marza\u0301","sequence":"additional","affiliation":[{"name":"Universitat Jaume I , , ,","place":["Castello\u0301, Spain, 12006"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,6,23]]},"reference":[{"issue":"1","key":"2026072709072305100_cit1","doi-asserted-by":"publisher","first-page":"148","DOI":"10.1021\/acscatal.7b02577","article-title":"Carbon-Increasing Catalytic Strategies\nfor Upgrading Biomass into Energy-Intensive Fuels and Chemicals","volume":"8","author":"Li","year":"2018","journal-title":"ACS Catal."},{"issue":"20","key":"2026072709072305100_cit2","doi-asserted-by":"publisher","first-page":"7818","DOI":"10.1039\/D2GC02956A","article-title":"Recent Developments in Electrode\nMaterials for the Selective Upgrade of Biomass-Derived Platform Molecules\ninto High-Value-Added Chemicals and Fuels","volume":"24","author":"Fan","year":"2022","journal-title":"Green\nChem."},{"issue":"5","key":"2026072709072305100_cit3","doi-asserted-by":"publisher","first-page":"2454","DOI":"10.1039\/D3GC04543A","article-title":"Electroreductive Upgradation of Biomass into High-Value\nChemicals and Energy-Intensive Biofuels","volume":"26","author":"Wang","year":"2024","journal-title":"Green\nChem."},{"key":"2026072709072305100_cit4","doi-asserted-by":"publisher","DOI":"10.1016\/j.rser.2024.114900","article-title":"Electrochemical Reduction\nHydrogenation, Hydrogenolysis and Dimerization of Bio-Derived Aldehydes:\nA Review","volume":"207","author":"Chen","year":"2025","journal-title":"Renewable Sustainable Energy Rev."},{"key":"2026072709072305100_cit5","doi-asserted-by":"publisher","DOI":"10.1002\/advs.202411964","article-title":"Recent Advances\nand Perspectives on Coupled Water Electrolysis for\nEnergy-Saving Hydrogen Production","volume":"12","author":"Li","year":"2025","journal-title":"Adv. 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Electrochem."},{"key":"2026072709072305100_cit21","doi-asserted-by":"publisher","first-page":"13158","DOI":"10.1021\/jacs.4c15821","article-title":"Driving Electrochemical\nOrganic Hydrogenations\non Metal Catalysts by Tailoring Hydrogen Surface Coverages","volume":"147","author":"Ciotti","year":"2025","journal-title":"J. Am. Chem. Soc."},{"issue":"2","key":"2026072709072305100_cit22","doi-asserted-by":"publisher","DOI":"10.1002\/advs.201700464","article-title":"Electrocatalysts\nfor Hydrogen Evolution in Alkaline Electrolytes: Mechanisms, Challenges,\nand Prospective Solutions","volume":"5","author":"Mahmood","year":"2018","journal-title":"Adv. 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Commun."},{"issue":"23","key":"2026072709072305100_cit26","doi-asserted-by":"publisher","first-page":"5245","DOI":"10.1002\/cssc.202101575","article-title":"Electroreductive\n5-Hydroxymethylfurfural Dimerization on Carbon Electrodes","volume":"14","author":"Kloth","year":"2021","journal-title":"ChemSusChem"},{"issue":"1","key":"2026072709072305100_cit27","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-022-35463-3","article-title":"Electroreductive Coupling\nof Benzaldehyde by Balancing the Formation and Dimerization of the\nKetyl Intermediate","volume":"13","author":"Yu","year":"2022","journal-title":"Nat. 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Eng."},{"issue":"22","key":"2026072709072305100_cit44","doi-asserted-by":"publisher","first-page":"12735","DOI":"10.1021\/acsomega.0c00227","article-title":"Potential-Dependent\nCompetitive Electroreduction of CO2 into CO and\nFormate on Cu(111) from an Improved H Coverage-Dependent Electrochemical\nModel with Explicit Solvent Effect","volume":"5","author":"Ou","year":"2020","journal-title":"ACS Omega"},{"issue":"12","key":"2026072709072305100_cit45","doi-asserted-by":"publisher","first-page":"7610","DOI":"10.1021\/acs.chemrev.8b00705","article-title":"Progress and Perspectives of Electrochemical CO2 Reduction\non Copper in Aqueous Electrolyte","volume":"119","author":"Nitopi","year":"2019","journal-title":"Chem. 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