Reduction Route Research Articles

Phenosafranine encapsulated mesoporous silica as efficient electrocatalyst for Cr(VI) reduction and its subsequent sensitive determination

This work presents an easy, highly specific, and sensitive route for the electrochemical reduction of Cr(VI) by phenosafranine (PSF+) integrated sulfonic acid functionalized mesoporous silica microspheres (MS-SO3−), denoted as PSF+-MS-SO3−. The synthesized material is characterized using various spectroscopic and microscopic methods. The glassy carbon electrode (GCE) is modified with this material (represented as GCE/PSF+-MS-SO3−) and employed for electroanalytical applications. The electrochemical characteristics of PSF+-MS-SO3− are established by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) techniques. Further, it is exploited for the electrocatalytic reduction of, Cr(VI). Superior electron transfer kinetics and stable electrochemical response for Cr(VI) are observed at the GCE/PSF+-MS-SO3− electrode. Moreover, the quantitative estimation of Cr(VI) at the GCE/PSF+-MS-SO3− done using linear sweep voltammetry (LSV). Dual linear calibration ranges (1 to 20 µM and 20 to 100 µM) is obtained from the LSV response. A low limit of detection (0.5 µM) and superior sensitivity (1.1 µA µM−1 cm−2) are recognized at this electrode. In addition, significant selectivity in the existence of other interfering ions is also shown by fabricated sensing scaffold. The precise measurement of Cr(VI) in spiked water samples with simple matrix is also demonstrated successfully with sufficient durability and reproducibility.

Clean Production of Hydrogen Peroxide: A Heterogeneous Solar‐Driven Redox Process

AbstractHydrogen peroxide is an essential chemical that is attracting strong attention for energy and environmental applications. However, the struggle between the growing market demand and the unsustainability of the conventional anthraquinone method motivates the exploration of alternative H2O2 production processes. Although several new production processes have been proposed, the environmental‐friendly solar‐driven H2O2 production attracts most attention because of the only inputs of water, oxygen, and light energy. The rational design of functional photo‐responsive catalysts promotes H2O2 production in the photocatalytic and photoelectrocatalytic approaches. These are, in general, achieved by facilitating the preferential adsorption of key intermediates of OOH*/OH*/O*, enhancing the light absorption, promoting the charge separation, and accelerating the surface charge transfer with selective number of involved charges. This review systematically summarizes strategies for photo(electro)catalysts toward H2O2 production via both the water oxidation and oxygen reduction pathways. Though the oxygen reduction route is perceived as more popular in the community, selective water oxidation is emerging as a convincing alternative. Furthermore, prevailing hypotheses, state‐of‐the‐art catalysts, critical challenges, and perspectives are discussed in depth. This review aims to enhance the comprehension of this research field and promote interest in sustainable H2O2 production.

Green and sustainable bio-synthesis of gold nanoparticles using Aspergillus Trinidadensis VM ST01: Heterogeneous catalyst for nitro reduction in water

In this study, a gold nanoparticles (GNPs) have been successfully fabricated by the bio reduction route using soil extract Aspergillus trinidadensis (VM ST01’ OL587588) fungi as a reducing and capping agent without any solvent interference. The GNPs were grown and stabilized by a two-step one-pot method, without any influence of chemical reactants. Characteristics of prepared GNPs were investigated using various microscopic and spectroscopic techniques. GNPs were roughly spherical in shape. Water dispersion study of GNPs has shown a stable dispersion in a broad range of 2–12 pH. The stirring and precursor salt concentration has influenced the kinetics involved in the fabrication process. Stoichiometric data has shown 3.5 × 1020 gold atoms per gram of biomass with diameters of around 35 nm, as determined with High-Resolution Transmission Electron Microscopy (HR-TEM). Zeta potential and Powder X-Ray Diffraction (P-XRD) studies have elucidated the crystalline nature of GNPs. Presence of participating functional groups were examined with Fourier Transform Infra-Red Spectroscopy (FT-IR). Synthesized GNPs were analyzed for surface morphology by Scanning Electron Microscope (SEM). The thermal stability of the lyophilized GNPs sample and capping of the particle were evaluated with Thermo-Gravimetric Analysis (TGA) and had a residual mass of 25% at 306 °C. The Aspergillus trinidadensis capped GNPs have been demonstrated as an efficient heterogeneous catalyst (AtGNHC) for the reduction of 4-Nitrophenol as a model substrate in water. An isolated yield (>95%) of the reduced product in 4 h has shown the effectiveness of the prepared catalyst.

In-situ constructing pearl necklace-shaped heterostructure: Zn2+ substituted Na3V2(PO4)3 attached on carbon nano fibers with high performance for half and full Na ion cells

Na3V2(PO4)3 (NVP) emerges as prospective cathode for sodium ion batteries. However, the poor electronic and ionic conductivity hinders its development. Traditional synthesis methods only allow ex-situ bonding between the NVP grains and carbon-based substrate, leading to unstable combination. Herein, a simultaneous modification strategy to optimize the morphological features and crystal construction of NVP system is proposed. The in-situ synthesized framework consisting of NVP and high conductive carbon nano fibers (CNFs) can efficiently elevate the electrochemical performance. A distinctive pearl necklace-shaped heterostructure is successfully constructed by electrospinning and carbon-thermal reduction routes. The necklace substrate is derived from the CNFs, possessing the unique unidimensional morphology and bridging well with each other to build a high conductive network. The Zn2+-substituted NVP grains with nano size are grown on the surface of the substrate. The shortened size provides short pathway for Na+ migration, resulting in the improved kinetic characteristics. Furthermore, the substitution of Zn2+ generates p-type doping to introduce favorable hole carriers, enhancing the ionic conductivity. The reduced band gap and migration energy barrier of Na+ for Zn2+ doped NVP is demonstrated by DFT calculations. Accordingly, the modified Zn0.07-ES-800 sample releases a high capacity of 117.5 mA h g−1 at 0.1C. It delivers a capacity of 92.3 mA h g−1 at 100C and maintains 72.7 mA h g−1 after 1000 cycles. Moreover, the Zn0.07-ES-800//Zn0.07-ES-800 full cell shows a high capacity of 94.4 mA h g−1 at 0.1C and keeps 80 mA h g−1 at 1C with a high retention of 95% after 70 cycles.

Zero-valent iron-peroxydisulfate as synergistic co-milling agents for enhanced mechanochemical destruction of 2,4-dichlorophenol: Coupling reduction with oxidation

Mechanochemical (MC) remediation with zero-valent iron (ZVI) as co-milling agent enables the non-combustion and solvent-free disposal of solid halogenated organic pollutants (HOPs) via solid-phase reaction, but suffers from incomplete dechlorination (especially for less chlorinated chemicals). Herein, a reduction-oxidation coupling strategy using ZVI and peroxydisulfate as synergistic (ZVI-PDS) co-milling agents was investigated, with 2,4-dichlorophenol (2,4-DCP) as probe contaminant. By revisiting the MC destruction process of 2,4-DCP by ZVI, the contribution of both reductive and oxidative routes is confirmed, and the inefficient •OH generation is addressed. With ball-to-material and reagent-to-pollutant mass ratios of 30:1 and 13:1, respectively, ZVI-PDS achieves higher dechlorination ratio (86.8%) for 2,4-DCP within 5 h, outcompeting sole ZVI (40.3%) or PDS (33.9%), due to the accumulation of numerous SO4•−. As suggested by a two-compartment kinetic model, the optimal ZVI/PDS molar ratio of 4:1 is determined, which balances the relative contribution of reductive/oxidative routes and leads to a maximum mineralization efficiency of 77.4%. The analysis on product distribution verifies the generation of dechlorinated, ring-opening and minor coupling products (with low acute toxicity). This work validates the necessity to couple reduction with oxidation in MC destruction for solid HOPs, and may provide information on reagent formulation.

A Review on Flash Sintering of Graphene Oxide Films: Mechanism and Recent Advances in the Field.

This review highlights the significance of flash sintering, a photothermal route, in reducing graphene oxide (GO) films. Essentially, extensive efforts are devoted to form graphene electrodes due to its distinctive properties, such as high surface area, excellent electrical conductivity, and optical transparency, owing to which it finds widespread use in energy storage devices, wearable electronics, sensors, and optoelectronics. Thus, rapidly rising market demands for these applications necessitate the need of a technique offering ease of manufacturability and scalability for production of graphene electrodes. The solution-processed graphene electrodes (SPGEs) are promising to fulfil these requirements. Particularly, SPGEs are fabricated by reducing GO film to graphene/reduced graphene oxide (rGO) by utilizing any reduction method, such as chemical, solvothermal, electrochemical, etc. Lately, flash sintering has garnered substantial attention as a promising reduction route for rapid, clean, and green production of graphene electrodes. This review briefly describes the underlying principle, mechanism, and parameters of flash sintering to develop an insight and advantages of this method over extensively used reduction methods. The review is a systematic summarization of the electrical, optical, and microstructural properties of rGO films/electrodes fabricated using this technique.

Regulation of the Tertiary N Site by Edge Activation with an Optimized Evolution Path of the Hydroxyl Radical for Photocatalytic Oxidation

Regulating the active sites to increase the yield of •OH is a specialized focus for pollutant photodegradation by g-C3N4-based photocatalysts. Herein, the tertiary N site was first tailored by edge activation to optimize the •OH evolution path. Ethyl alcohol and cyano group comodified g-C3N4 was first fabricated via a facile one-pot thermal copolymerization route to achieve a high yield of •OH. The as-prepared N20–CN exhibited first-class photocatalytic oxidation ability in the degradation of phenol (k40 min is 26.3 times higher than that of BCN). Both experimental results and DFT calculations disclose that the tertiary N site with increased electron density via synergy of the two groups realizes not only the oxygen reduction route mediated with •O2– but also the in situ conversion of H2O2 between high production and strong reduction, governing the O2 → •O2– → H2O2 → •OH optimal evolution path with a high yield of •OH. This paper provided a theoretical basis for the development of a superactive g-C3N4-based photocatalyst and optimization of •OH evolution paths via the edge activation strategy for solar-driven photochemical applications.

Discovery and Engineering of an Ene‐reductase for Kinetic Resolution and Cascade Reduction of Hajos‐Parrish/Wieland‐Miescher Ketones

AbstractEne‐reductase (ERED)‐catalyzed asymmetric reduction of α,β‐unsaturated ketones is an attractive method in organic synthesis. Through the discovery and further structure‐guided protein engineering of BsER, an ERED from Bacillus subtilis, the selective bio‐reduction of the well‐known building blocks Hajos‐Parrish ketone (HPK, 1 a) and Wieland‐Miescher ketone (WMK, 1 b) was achieved in this study. The optically pure (R)‐HPK ((R)‐1 a) and (R)‐WMK ((R)‐1 b) with corresponding >99% and 98% enantiomeric excess (ee) values were obtained by kinetic resolution of the racemic substrates. To the best of our knowledge, this is the first example of ERED mediated kinetic resolution of rac‐HPK and rac‐WMK. In addition, the reduction products cis‐7a‐methylhexahydro‐1H‐indene‐1,5(4H)‐dione (cis‐2 a) and cis‐8a‐methylhexahydronaphtha‐ lene‐1,6(2H,5H)‐dione (cis‐2 b) with high diastereomeric ratios (dr) were also obtained. We also developed four routes of biocatalytic cascade reduction involving BsER and ketoreductases (KREDs). Using optimized ERED‐KRED and KRED‐ERED cascades, (S)‐HPK ((S)‐1 a) and (S)‐WMK ((S)‐1 b) could be reduced stepwise, yielding the bioactive products all with >91% purity. This study presents a biocatalytic strategy for the kinetic resolution and cascade reduction of HPK and WMK (1 a and 1 b).

The Chemistry of Vanadium bis‐Phenolate NHC Complexes in Three Oxidation States

AbstractTwenty‐one vanadium bis‐phenolate benzimidazolylidene complexes, spanning three oxidation states, have been investigated. Special emphasis is placed on their salt metathesis reactivity and the accessibility of the +IV oxidation state by reductive or oxidative routes, starting from vanadium(V) or vanadium(III) respectively. While the reductive route is highly dependent on the reducing agent and starting material used, the oxidative route gives clean access to vanadium(IV) dihalide complexes. The low‐valent vanadium(III) complexes are excellent precursors for salt metathesis reactions which lead to the isolation of a rare vanadium(III) NHC alkyl complex. All new complexes have been characterized by (paramagnetic) 1H NMR and 51V NMR, UV–VIS, IR and EPR spectroscopy as well as elemental analysis. Cyclic voltammetry has been performed in selected cases to study the influence of imido or phenolate supporting ligands towards the redox‐potential of the vanadium(V/IV) redox couple compared to the parent oxo‐chlorido complex A.

Advanced physical model of hydrothermic reduction of iron ore pellets by dissociated 2H+ ionic gas in the shaft furnace

ABSTRACT Development of various alternative routes for the direct reduction of iron-ore (DRI) and production of sponge irons becomes a necessity today to reduce carbon dioxide (CO2) gas emissions in industrial iron & steel (I&S) making processes. Therefore, the main objective of this work is focused to reduce the carbon footprint in DRI production by eliminating fossil fuel consumption. The reduced iron could be used to melt in the electric arc furnace (EAF) to produce liquid steel by minimising direct scrap addition. Indeed, this paper shows an advanced physical model of a hydrogen fuel shaft furnace for the direct reduced iron-making process by fundamental development of technology with essential modifications in its working principle. This processing technology is hypothetically designed with knowledge of theoretical literature inputs and wisdom of iron and steel-making experience. In this model of a shaft furnace, a scientific approach is designed based on the dissociation of molecular-hydrogen gas (H2+) obtained by water electrolysis and ionisation of the hydrogen gas (2H+) and is incorporated for a high degree of gas adsorption and metallisation during chemical reduction of iron ore (Fe2O3) pellets. The steps involved in the working principle of the new design shaft furnace are simulated and modelled suitably for the existing Midrex furnace operation, which is generally used for DRI production. This approach could be tried using 100% dissociated hydrogen ionic gas (2H+, H+) for future direct reduced iron making by water electrolysis and hydrogen ionisation. Moreover, the reformed reducing gases (CH4–H2–CO) used in the Midrex process can be replaced by the ionised hydrogen gases as an advancement.

One-step synthesized Bi5O7I for extremely low-temperature CO2 electroreduction

This work provides a scalable, one-step ultrasound-assisted reduction route, which prepares needle-tip Bi 5 O 7 I in a large quantity at ambient condition. At -50℃, the Bi 5 O 7 I-based flow cells can operate with a formate selectivity >90% and a large partial current density.

SO2-tolerant mesoporous iron oxide supported bimetallic single atom catalyst for methanol removal

Among the single-atom catalysts (SACs), the bimetallic single-atom catalysts play an increasingly promising role in the oxidative removal of volatile organic compounds (VOCs) due to their high efficiency. However, it remains a significant challenge to resist SO2 poisoning in industrial applications. In this work, we report (i) the synthesis of three-dimensionally ordered mesoporous Fe2O3-supported bimetallic AuPt single-atom (denote as Au1Pt1/meso-Fe2O3) catalyst via a modified polyvinyl alcohol-protected reduction route; (ii) catalytic performance of the catalysts for methanol oxidation; and (iii) catalytic and SO2-resistant mechanism. It was found that compared with Pt1/meso-Fe2O3 and Ptnp/meso-Fe2O3, Au1Pt1/meso-Fe2O3 exhibited better catalytic activity for methanol combustion, with the temperature at 90% methanol conversion, TOFnoble metal at 120 °C, and apparent activation energy being 137 °C at a space velocity of 20 000 mL g–1 h–1, 6.51 × 10–2 s–1, and 36 kJ mol− 1, respectively. The enhanced activity was associated with the improved reducibility, methanol adsorption ability, and strong interaction between noble metal and support. The reaction pathway was deduced to follow a sequence of methanol → methoxy species → formaldehyde → formic acid → CO2 and H2O. Furthermore, the order of SO2 resistance was Au1Pt1/meso-Fe2O3 > Pt1/meso-Fe2O3 > Ptnp/meso-Fe2O3. The good SO2 resistance of the Au1Pt1/meso-Fe2O3 catalyst was attributed to the Au−Pt bimetallic single atoms uniformly dispersed on the meso-Fe2O3 with the strong ability of sulfate decomposition and the protection of the active sites by meso-Fe2O3 as a sacrificial site. This work presents a novel way for developing high-performance catalysts for VOCs elimination in the presence of SO2.

Low carbon optimal planning of the steel mill gas utilization system

Decarbonization of the steelmaking industry is imperative in achieving the carbon neutrality target. This paper proposes a two-stage low carbon robust planning method for the steel mill gas utilization system (SMGUS), which is the major CO2 emission source of the conventional blast furnace route based-steelmaking plant. The planning aims to find the optimal installed capacities and relevant deployment time of multiple low-carbon technologies, such as renewable energy, energy storage, hydrogen energy and carbon capture & utilization, so that the demand of steel production can be met in an economically competitive and environmentally friendly way. Case studies are carried out on the low-carbon planning of a steelmaking plant with annual production of 1.5 million tons of crude steel, in which different carbon market conditions and CO2 reduction routes are considered. The results show that the low carbon planning can reduce the CO2 emissions to 1.22 tons per ton of steel by 2045–2050 through the proper deployment of the low carbon technologies. The CO2 emissions can be further reduced to 0.31 tons per ton of steel if the BF-BOF process is replaced by H2-DRI and EAF technologies. This paper presents an effective planning method for the decarbonization of steelmaking plant.

Construction of PEGylated chlorin e6@CuS-Pt theranostic nanoplatforms for nanozymes-enhanced photodynamic-photothermal therapy

Multifunctional nanoagents with photodynamic therapy (PDT) and photothermal therapy (PTT) functions have shown great promise for cancer treatment, while the design and synthesis of efficient nanoagents remain a challenge. To realize nanozyme-enhanced PDT-PTT combined therapy, herein we have synthesized the Ce6@CuS-Pt/PEG nanoplatforms as a model of efficient nanoagents. Hollow CuS nanospheres with an average diameter of ∼ 200 nm are first synthesized through vulcanization using Cu2O as the precursor. Subsequently, CuS nanospheres are surface-decorated with Pt nanoparticles (NPs) as nanozyme via an in-situ reduction route, followed by modifying the DSPE-PEG5000 and loading the photosensitizer Chlorin e6 (Ce6). The obtained Ce6@CuS-Pt/PEG NPs exhibit high photothermal conversion efficiency (43.08%), good singlet oxygen (1O2) generation ability, and good physiological stability. In addition, Ce6@CuS-Pt/PEG NPs show good catalytic performance due to the presence of Pt nanozyme, which can effectively convert H2O2 to O2 and significantly enhance the production of cytotoxic 1O2. When Ce6@CuS-Pt/PEG NPs dispersion is injected into mice, the tumors can be wholly suppressed owing to nanozyme-enhanced PDT-PTT combined therapy, providing better therapeutic effects compared to single-mode phototherapy. Thus, the present Ce6@CuS-Pt/PEG NPs can act as an efficient multifunctional nanoplatform for tumor therapy.

Unravelling the role of reactive oxygen species in ultrathin Z-scheme heterojunction with surface zinc vacancies for photocatalytic H2O2 generation and CTC degradation

Photo-induced reactive oxygen species (ROS) produced by molecular oxygen activation and oxidization of H2O/OH− during photocatalytic reaction are extremely important in environmental remediation. Herein, a dual pathway to improve ROS formation was designed through establishing ultrathin 2D/2D Z-scheme heterojunction and defect engineering in O-doped g-C3N4/ZnIn2S4-Zn (ZIS-Z/OCN) composite. The results of experiment and density functional theory (DFT) calculation indicate that the charge-carriers are spatially separated in composite driven by different work functions and ultrathin 2D/2D interface, boosting charge-transfer efficiency from 42.05 % (ZnIn2S4-Zn) to 59.93 % (40ZIS-Z/OCN). Benefiting by this fact, improving molecular oxygen activation capacity can induce more ROS generation. In consequence, 40ZIS-Z/OCN reveals optimal chlortetracycline hydrochloride (CTC) removal efficiency (88.43 %) and hydrogen peroxide (H2O2) yield (168.67 μmol/L) under visible light irradiation. The results of control experiments show that H2O2 is generated via two-step electron reduction route and singlet oxygen (1O2) conversion. This study provides new views on the construction of cost-effective and reusable photocatalysts for environmental remediation and energy conversion.

Adsorption and kinetic studies of chromium (VI) removal using Ag2Cu2O3 nanoparticles

Abstract This study reports the removal of chromium (VI) from waste aqueous medium using disilver-dicopper oxide nanoparticles (Ag2Cu2O3 NPs) as adsorbent, which were synthesized by adopting reduction route of chemical method and stabilized by emulsifier (sodium dodecyl sulfate [SDS]). Synthesized nanoparticles were further characterized using different analysis techniques such as UV–Vis for the detection of NPs via Λmax and their point-zero charge (pzc) determination also done. Whereas, FTIR and XRD were done to determine the functional groups, crystal plane (tetragonal) and crystallite size (15.19 nm) of Ag2Cu2O3 NPs respectively. SEM was used with EDX for morphology and elemental confirmation respectively. The synthesized nanoparticles were then employed for the adsorptive removal of chromium (VI) (Cr(VI)). Different parameters including pH, temperature, agitation time, adsorbate and adsorbent’s concentration were also studied. At optimized conditions, 0.5 g adsorbent, 40 ppm concentration of Cr(VI) solution along with 1 h agitation time were studied. Maximum observed adsorption and chromium removal efficiency was 96.66319 %. Four adsorption isotherms namely; Freundlich, Langmuir, Temkin and Harkins-Jeura were employed from which Freundlich adsorption model gives best fitting on experimental results. The kinetic modelling had shown that adsorption process follows second order kinetics. The thermodynamic studies of the adsorptive removal of Cr(VI) also evaluated. The Ag2Cu2O3 NPs adsorbent’s reusability were also determined. The study had proven that Ag2Cu2O3 nanoparticles are efficient adsorbents for the removal of Cr(VI).

Ligand-Assistant Iced Photocatalytic Reduction to Synthesize Atomically Dispersed Cu Implanted Metal-Organic Frameworks for Photo-Enhanced Uranium Extraction from Seawater.

Uranium extraction from natural seawater is one of the most promising routes to address the shortage of uranium resources. By combination of ligand complexation and photocatalytic reduction, porous framework-based photocatalysts have been widely applied to uranium enrichment. However, their practical applicability is limited by poor photocatalytic activity and low adsorption capacity. Herein, atomically dispersed Cu implanted UiO-66-NH2 (Cu SA@UiO-66-NH2 ) photocatalysts are prepared via ligand-assistant iced photocatalytic reduction route. N-Cu-N moiety acts as an effective electron acceptor to potentially facilitate charge transfer kinetics. By contrast, there exist Cu sub-nanometer clusters by the typical liquid phase photoreduction, resulting in a relatively low photocatalytic activity. Cu SA@UiO-66-NH2 adsorbents exhibit superior antibacterial ability and improved photoreduction conversion of the adsorbed U(VI) to insoluble U(IV), leading to a high uranium sorption capacity of 9.16mg-U/g-Ads from natural seawater. This study provides new insight for enhancing uranium uptake by designing SA-mediated MOF photocatalysts.

Research progress in the preparation of iron by electrochemical reduction route without CO2 emissions

Research progress in the preparation of iron by electrochemical reduction route without CO2 emissions

NiFeZnP Nanosheets with Enriched Phosphorus Vacancies for Supercapattery Electrodes

Designing and fabricating outstanding electrode materials via simple preparation routes are viable ways for improving the performance of electrochemical supercapacitors. We report on the synthesis of NiFeZn phosphide interconnected nanosheets with abundant phosphorus vacancies (Pv-NiFeZnP) via a facile reduction route at room temperature. The fabricated Pv-NiFeZnP was fully characterized using energy-dispersive spectroscopy, field emission scanning electron microscopy, electron paramagnetic resonance, and X-ray photoelectron spectroscopy techniques. Owing to the porous interconnected nanosheet structure and the superior stability enabled by the direct binder-free growth on Ni foam, the Pv-NiFeZnP electrode, with optimized phosphorus vacancy formation, exhibits a superb electrochemical performance of 631.8 mC/cm2 (equivalent to 1579.5 mF/cm2), which is significantly higher than those reported in the literature. Also, the Pv-NiFeZnP||activated carbon asymmetric device exhibits a very high Coulombic efficiency (∼100%) and excellent long-term stability (98.8% capacity retention after 7500 cycles). The fabricated device can deliver 122.1 μWh/cm2 energy density at a power density of 750 μW/cm2. The fabricated NiFeZnP electrode is therefore a promising candidate for supercapacitor applications.

A microwave-assisted and efficient reduction protocol for the synthesis of alkyl-substituted [2.2]-paracyclophanes

[2.2]-Paracyclophane derivatives have been promising platforms for applications in biology and materials science. To access pure derivatives thereof, a safe and non-toxic synthetic method for 4- n-propyl-[2.2]-paracyclophane is developed via a microwave-assisted and NH2NH2/KOH reduction route. We introduce microwave-assisted acylation for a synthesis that successfully improves the yield and reduces the reaction time. Notably, an exploration of the length and number of the alkyl chains on the [2.2]-paracyclophane ring did not significantly affect the outcome of this reaction. We synthesized 4- n-butyl-[2.2]-paracyclophane and 4,12-dipropyl-[2.2]-paracyclophane via our protocol with high yields. The regioselectivity of the second electrophilic substitution on 4- n-propyl-[2.2]-paracyclophane occurs at the para position of the less substituted phenyl ring.