Conditions In High Yields Research Articles

The synthesis of Fe3O4@SiO2-NNO-CuII nanocatalyst and investigation of its application in the synthesis of imidazo[1,2-a]pyridines

In this study, a tridentate Schiff base ligand obtained from the condensation of salicylaldehyde and 3-amino-1,2,4 triazole was covalently immobilized on the surface of 3-chloro-trimethoxysilane-functionalized magnetic nanoparticles. This nitrogen and oxygen-rich compound provides donor arms for the coordination of copper ions. The prepared nanocatalyst (Fe3O4@SiO2-NNO-CuII) has been characterized by various techniques including FT-IR, EDX, SEM, VSM, XRD and ICP analysis and used as an efficient recyclable catalyst for the synthesis of imidazo[1,2-a]pydidines. Imidazo[1,2-a]pyridine products were obtained through the coupling reaction of substituted benzaldehydes, 2-aminopyridine derivatives and phenylacetylene under solvent-free conditions in high yields and short reaction times.

Photocatalytic Three-Component Acylcarboxylation of Alkenes with CO2.

γ-Keto acid is a valuable chemical motif in a wide range of fields including organic, biological, and medicinal chemistry. However, its single-step synthesis is challenging because of the mismatch of the carbonyl polarity and low tolerance of carboxylic acids. Herein, we report the single-step syntheses of γ-keto acids using alkenes and CO2. Our photocatalytic system enabled the transformation of alkenes under mild conditions in high yields (up to 95%) with broad substrate generality (35 examples).

Soybean seed yield, protein, and oil concentration for a modern and old genotype under varying row spacings

Progress in soybean (Glycine max L.) breeding has led to a reduction in optimal seeding rates due to enhanced branching capacity over time. However, less is known about the changes in canopy architecture between old and modern soybean genotypes at varying row spacing and their impact on yield and seed quality through the main stem and branches. Therefore, this study aimed to i) evaluate yield and seed quality responses of an old and modern soybean genotype at different row spacings and ii) examine the yield and seed quality of branches and the main stem. Trials were conducted in Kansas (United States, US) during 2020 and 2021, comparing two genotypes (old, released in 1980, and modern, released in 2013) at four row spacings (0.19, 0.38, 0.76, and 1.52 m) under rainfed conditions. Seed yield and quality (protein and oil concentrations, %) were assessed at the end of each growing season. In 2021, both genotypes had low and similar yields at all row spacings (averaging 2481 kg ha−1) with 2.5 % less protein on branches compared to the main stem. However, 2022 resulted in a high-yielding environment, with the modern yielding 50 % more (3584 kg ha−1) than the old (2315 kg ha−1) genotype in narrow row spacings (<0.38 m). Additionally, the modern genotype showed a three-fold greater contribution to yield from branches (1113 kg ha−1) relative to the old genotype (379 kg ha−1). Despite the high yields observed in narrow rows, the modern genotype maintained protein levels. These results highlight the importance of row spacing as a key management practice for improving yield while maintaining protein levels in high yield conditions.

Insights into microwave‐promoted synthesis of 3‐methyl‐4‐phenyl‐4,9‐dihydro‐1H‐pyrazolo[3,4‐d][1,2,4]triazolo[1,5‐a]pyrimidine derivatives catalyzed using new Pd (II),Cu (II),VO (II), and Ag(I) complexes as a heterogeneous catalyst and computational studies

Four novel Pd (II), Cu (II), VO (II), and Ag(I) complexes were prepared from benzimidazole ligand through bidentate chelating mode. Alternative spectral and analytical tools were applied to elucidate their structural and molecular formulae. This study was extended to investigate stability and stoichiometry of complexes in solution, using standard methods. In addition, the best atomic distribution within structural forms was obtained via the density functional theory (DFT) method. This computational study fed us with significant physical characteristics for differentiation. Also, DFT/time‐dependent DFT computations were performed applying (B3LYP/6‐311++G[d,p]/aug‐cc‐pVTZ/aug‐cc‐pVTZ‐PP) level in order to investigate the electronic behavior of the compounds. These results demonstrated good agreement with the experimental data. Computational data discriminate Pd (II) complex by some physical features, which may be promising in the catalytic field. This complex was selected to play a catalytic function to synthesize 3‐methyl‐4‐phenyl‐4,9‐dihydro‐1H‐pyrazolo[3,4‐d][1,2,4]triazolo[1,5‐a]pyrimidine derivatives using microwave irradiation in a one‐pot reaction. The catalyst was selected for this application based on the history of Pd (II) complexes and the properties expected theoretically. A condensation reaction for 3‐methyl‐5‐pyrazolone, aromatic aldehyde, and 5‐aminotetrazole was carried out under mild reaction conditions by microwave irradiation. All reaction conditions were optimized among those variable Lewis acid catalysts in comparison with our new complexes. DOBPAPd catalyst displayed superiority in overall trials with high yield, short time, and green conditions (solvent H2O/EtOH). Also, the recovery of hetero catalyst was succeeded and reused by the same efficiency up to five times after that the efficiency was reduced. The mechanism of action was proposed based on the ability of Pd (II) for adding extra‐bonds over z‐axis and supported by theoretical aspects.

Thermal imaging can reveal variation in stay-green functionality of wheat canopies under temperate conditions.

Canopy temperature (CT) is often interpreted as representing leaf activity traits such as photosynthetic rates, gas exchange rates, or stomatal conductance. This interpretation is based on the observation that leaf activity traits correlate with transpiration which affects leaf temperature. Accordingly, CT measurements may provide a basis for high throughput assessments of the productivity of wheat canopies during early grain filling, which would allow distinguishing functional from dysfunctional stay-green. However, whereas the usefulness of CT as a fast surrogate measure of sustained vigor under soil drying is well established, its potential to quantify leaf activity traits under high-yielding conditions is less clear. To better understand sensitivity limits of CT measurements under high yielding conditions, we generated within-genotype variability in stay-green functionality by means of differential short-term pre-anthesis canopy shading that modified the sink:source balance. We quantified the effects of these modifications on stay-green properties through a combination of gold standard physiological measurements of leaf activity and newly developed methods for organ-level senescence monitoring based on timeseries of high-resolution imagery and deep-learning-based semantic image segmentation. In parallel, we monitored CT by means of a pole-mounted thermal camera that delivered continuous, ultra-high temporal resolution CT data. Our results show that differences in stay-green functionality translate into measurable differences in CT in the absence of major confounding factors. Differences amounted to approximately 0.8°C and 1.5°C for a very high-yielding source-limited genotype, and a medium-yielding sink-limited genotype, respectively. The gradual nature of the effects of shading on CT during the stay-green phase underscore the importance of a high measurement frequency and a time-integrated analysis of CT, whilst modest effect sizes confirm the importance of restricting screenings to a limited range of morphological and phenological diversity.

Production of Hydrogen with Ruminal Microbiota: Finding Culture Conditions for High Yields

Hydrogen is ideal for replacing fossil fuels because upon combustion it generates only water. Dark fermentation (DF) from lignocellulose might be a competitive process for hydrogen production at the industrial scale. However, lignocellulose must be pretreated to obtain fermentable sugars, which is costly and creates pollution. Microorganisms from bovine rumen efficiently degrade lignocellulose. Unfortunately, they have scarcely been explored for the production of hydrogen. Therefore, deeper studies on the culture conditions have to be undertaken to understand the behavior of microbial consortia from the rumen of bovines (MCRB) during hydrogen production. In this work, we evaluated the production of hydrogen by DF with MCRB by varying the incubation time, two culture media (MB and Rhodospirillaceae), headspace (40 and 80 mL), and thermal treatment. It was found that the production of hydrogen was maximum at 16 h MCRB incubation in MB. An amount of 80 mL headspace resulted in a threefold production of hydrogen as compared to 40 mL; the MCRB without heat treatment had a higher H2 yield. The production of hydrogen with 32 MCRB was highly variable, ranging between 21 and 696 mL. Our findings show a different perspective on the treatment of MCRB for the production of hydrogen and give insights on the impact of the culture conditions for increasing hydrogen production.

Efficient Solvent-Free Synthesis of Indolizines Using CuBr Catalyst from Pyridine, Acetophenone, and Electron-Deficient Alkenes.

Herein, we have developed a new approach for the synthesis of indolizine via Cu-catalyzed reaction of pyridine, acetophenone, and nitroolefin under mild conditions in high yields. This reaction involved the formation of C-N and C-C bonds and new indolizine compounds with high stereoselectivity and excellent functional group tolerance.

High-efficiency thermal reduction of CO2 to high-valued carbon nanotubes

To reduce the amount of carbon dioxide (CO2) already emitted into the atmosphere, various carbon capture, utilization, and storage (CCUS) technologies have been developed for climate and economic reasons in recent years. However, the state of art CCUS techniques suffer from deficiencies such as high cost, low yield, and harsh and discontinuous production conditions. In this work, we report a new thermal reduction method for continuously conversing CO2 to methane (CH4) by introducing sodium borohydride (NaBH4) as a reductant under catalyst-free conditions. Experimental results show that CO2 can be fully captured and converted to CH4 and carbon monoxide (CO) and the selectivity efficiency of CO2 to CH4 can be achieved to be as high as 90% with the optimization of experimental conditions. Such a result originates from the high activity of NaBH4 and high selectivity of the thermal reduction of CO2. To demonstrate one of the potential usages of the reduction products, we integrated the thermal reduction of CO2 with the production of carbon nanotubes (CNTs). As long as CO2 is supplied at the source end, the reduction products can undergo catalytic decomposition to produce a CNT fiber or film continuously at the final end. The present technique is featured with simple equipment setup, low cost, and continuous thermal reduction, thus providing a new pathway for the large-scale conversion of CO2 into high-valued products for wide applications.

Direct synthesis of acyl fluorides from carboxylic acids using benzothiazolium reagents.

2-(Trifluoromethylthio)benzothiazolium triflate (BT-SCF3) was used as deoxyfluorinating reagent for the synthesis of versatile acyl fluorides directly from the corresponding carboxylic acids. These acyl fluorides were reacted with amines in a one-pot protocol to form different amides, including dipeptides, under mild and operationally simple conditions in high yields. Mechanistic studies suggest that BT-SCF3 can generate acyl fluorides from carboxylic acids via two distinct pathways, which allows the deoxyfluorinating reagent to be employed in sub-stoichiometric amounts.

Synthesis of spiro-oxindole-based chemosensor for detection of Hg2+ ions using SBA-Pr-N-IS-Bu-SO3H

Spiro-oxindoles were prepared efficiently via multicomponent reactions (MCRs) for finding the new chemosensors. Also, the use of the efficient nanocatalysts based on SBA-15 in these reactions are so important. Therefore, the functionalization of SBA-15 by different organic compounds are common to produce new efficient nanocatalysts. Herein, SBA-Pr-N-Is-Bu-SO3H as an efficient nanoporous catalyst was applied in the synthesis of (5,6,7,8-tetrahydro-chromene)-4,3′-spirocyclic oxindoles through the three-component reaction of isatin derivatives, malononitrile and dimedone under reflux conditions in high yield and short reaction time. Among all spiro-oxindole derivatives, 2-amino-7,7-dimethyl-5′-nitro-2′,5-dioxo-5,6,7,8-tetrahydro-spiro[chromen-4,3′-indoline]-3-carbonitrile was investigated in fluoresence spectroscopy. According to the obtained results it was observed that in the presence of various cations such as, K+, Ca2+, Na+, Cu2+, Zn2+, Cr3+, Fe3+, Fe2+, Mn2+, Co2+, Al3+, Pb2+, Ag+, Cd2+, Ni2+, Hg2+ and Mg2+, it can selectively detect Hg2+ ion and increase the emission intensity. Its calculated detection limit was 4.6 × 10−7 M, which can be considered a good value. Also, in order to determine the stoichiometric ration for ligand and Hg2+ ion, Job's plot test was performed and the ratio was 1:2.

Climate and disease: tackling coffee brown-eye spot with advanced forecasting models.

Climate influences the interaction between pathogens and their hosts significantly. This is particularly evident in the coffee industry, where fungal diseases like Cercospora coffeicola, causing brown-eye spot, can reduce yields drastically. This study focuses on forecasting coffee brown-eye spot using various models that incorporate agrometeorological data, allowing for predictions at least 1 week prior to the occurrence of disease. Data were gathered from eight locations across São Paulo and Minas Gerais, encompassing the South and Cerrado regions of Minas Gerais state. In the initial phase, various machine learning (ML) models and topologies were calibrated to forecast brown-eye spot, identifying one with potential for advanced decision-making. The top-performing models were then employed in the next stage to forecast and spatially project the severity of brown-eye spot across 2681 key Brazilian coffee-producing municipalities. Meteorological data were sourced from NASA's Prediction of Worldwide Energy Resources platform, and the Penman-Monteith method was used to estimate reference evapotranspiration, leading to a Thornthwaite and Mather water-balance calculation. Six ML models - K-nearest neighbors (KNN), artificial neural network multilayer perceptron (MLP), support vector machine (SVM), random forests (RF), extreme gradient boosting (XGBoost), and gradient boosting regression (GradBOOSTING) - were employed, considering disease latency to time define input variables. These models utilized climatic elements such as average air temperature, relative humidity, leaf wetness duration, rainfall, evapotranspiration, water deficit, and surplus. The XGBoost model proved most effective in high-yielding conditions, demonstrating high precision and accuracy. Conversely, the SVM model excelled in low-yielding scenarios. The incidence of brown-eye spot varied noticeably between high- and low-yield conditions, with significant regional differences observed. The accuracy of predicting brown-eye spot severity in coffee plantations depended on the biennial production cycle. High-yielding trees showed superior results with the XGBoost model (R2 = 0.77, root mean squared error, RMSE = 10.53), whereas the SVM model performed better under low-yielding conditions (precision 0.76, RMSE = 12.82). The study's application of agrometeorological variables and ML models successfully predicted the incidence of brown-eye spot in coffee plantations with a 7 day lead time, illustrating that they were valuable tools for managing this significant agricultural challenge. © 2024 Society of Chemical Industry.

14N to 15N Isotopic Exchange of Nitrogen Heteroaromatics through Skeletal Editing.

The selective modification of nitrogen heteroaromatics enables the development of new chemical tools and accelerates drug discovery. While methods that focus on expanding or contracting the skeletal structures of heteroaromatics are emerging, methods for the direct exchange of single core atoms remain limited. Here, we present a method for 14N → 15N isotopic exchange for several aromatic nitrogen heterocycles. This nitrogen isotope transmutation occurs through activation of the heteroaromatic substrate by triflylation of a nitrogen atom, followed by a ring-opening/ring-closure sequence mediated by 15N-aspartate to effect the isotopic exchange of the nitrogen atom. Key to the success of this transformation is the formation of an isolable 15N-succinyl intermediate, which undergoes elimination to give the isotopically labeled heterocycle. These transformations occur under mild conditions in high chemical and isotopic yields.

A straightforward and rapid synthesis of polydithioacetals in the presence of chlorodimethylsilane

Rapid synthesis of polydithioacetals (PDTAs) under mild conditions in high yields and varying molecular weights in the presence of chlorodimethylsilane (CDMS) is reported.

Dibenzoylperoxide‐Mediated Oxidative α‐Thio/Seleno‐Cyanation of β‐Ketoesters and Oxindoles

AbstractWe herein report a protocol for the α‐thio‐ and α‐seleno‐cyanation of different cyclic β‐ketoesters and oxindoles by using NaSCN or KSeCN as easily accessible inorganic nucleophilic S(e)CN sources under oxidative conditions. Key to success for both transformations is the use of dibenzoylperoxide as an oxidant allowing for the coupling of two inherently nucleophilic species under operationally simple conditions in high yields and with broad functional group tolerance.

An ICP-MS study on metal content in biodiesel and bioglycerol produced from heated and unheated canola oils

This study addresses the challenges of biodiesel production costs and waste oil disposal by investigating the use of low-cost waste oil as a feedstock. The impact of heating temperature on biodiesel yield and trace metal levels is examined using response surface methodology (RSM). Optimal conditions for high biodiesel yields (95–98%) from canola oil are determined with a methanol/oil ratio of 12:1, 1 wt% catalyst, and 60-min reaction time. For crude bioglycerol, the optimal conditions involve a methanol/oil ratio of 4.25:1, 2.93 wt% catalyst, and 119.15-min reaction time. Elemental analysis reveals the presence of high-concentration metals like Cu and Zn and low-concentration ones such as Pb, As, Se, and Zr in both oil feedstocks and their respective biodiesel and bioglycerol products. The study demonstrates that thermal stress on canola oil significantly impacts biodiesel and bioglycerol yields and trace metal levels during the transesterification process. The findings contribute to enhancing cost-effectiveness and environmental sustainability in biodiesel production.

Copper(II)-Catalyzed Enantioselective Aza-Friedel-Crafts Reaction of Indoles with Isatin-Derived N-Boc-Ketimines.

The copper(II)-catalyzed enantioselective aza-Friedel-Crafts reaction of indoles with isatin-derived N-Boc-ketimines was developed by using tunable chiral O-N-N tridentate ligands derived from BINOL and proline. In general, the reaction afforded chiral 3-indolyl-3-aminooxindoles under mild conditions in high yields (83-97%) with excellent ee (69-99%).

Using Triazolobenzodiazepine as the Cyclic Imine in Various Types of Joullié-Ugi Reactions.

The triazolobenzodiazepine as a cyclic imine was employed in a variety of Joullié-Ugi reactions, and three new families of unique triazolobenzodiazepine connected to carboxamide and tetrazole products were synthesized via a three-component reaction of the cyclic imine and isocyanides with each species of a carboxylic acid/water/TMSN3 under mild conditions in high yields. Furthermore, triazolobenzodiazepine imine was used in an interesting strategy based on the modified Ugi reaction (pseudo-Joullié-Ugi reaction) of cyclic imines with an isocyanide and acetylenedicarboxylates under catalyst-free conditions for the synthesis of triazolobenzodiazepine-fused pyrroles. Mechanistic investigation reveals that triazolobenzodiazepine-fused pyrroles have been generated via a surprising route. Significantly, the use of triazolobenzodiazepine in the Joullié-Ugi, azido-Joullié-Ugi, and pseudo-Joullié-Ugi reactions of a broad scope of biological scaffolds occurred under mild, simple conditions without any catalyst.

The effectiveness of using some criteria for determining adaptability on the example of winter rye cultivars

Background. For most regions of Russia, winter rye is an indispensable grain and fodder cereal. Recently, winter rye crops have been declining. It is possible to improve this situation by releasing cultivars that ensure consistently high grain productivity under various growing conditions. Therefore, measuring the level of adaptability for yields in different mathematical quantities using a variety of methods is an urgent need. Materials and methods. For an unprejudiced assessment of winter rye cultivars, the following adaptability parameters were calculated and analyzed: the intensity coefficient (I) and constancy of the stability index (Y) according to Udachin and Golovchenko; stability index (IS) according to Hangildin; range breadth (Jsp) according to Eberhart and Russell; breeding value (Sc) according to Hangildin; responsiveness coefficient (Cr.) according to Zykin; genotypic effect (Ɛi) according to Guryev; equalization coefficient (B) according to Dospekhov; multiplicativity coefficient (KM) according to Dragavtsev; and reaction effect (Er.) according to Novokhatin. Field experiments and the study of 8 winter rye cultivars were carried out according to VIR’s guidelines in 2012–2017. Results and conclusion. A significant variation was found in grain yield; it was induced by the high contribution of the “year” factor (79.4 %). The best conditions for higher yields were formed in 2012 and 2015. An analysis of the six-year average yield showed that cvs. ‘Rushnik 2’, ‘Bereginya’, and ‘Novaya Era’ exceeded ‘Ilmen’ by 5–22 %. It was shown that among the selected ten indicators, worth attention were the multiplicativity coefficient, the stability index, the breeding value index, the reaction effect of a cultivars, and the range breadth index: they established the adaptability level of a cultivar with higher statistical significance. Cvs. ‘Novaya Era’, ‘Yanrarnaya, ‘Bereginya’, and ‘Vavilovskaya’ from the analyzed set demonstrated high adaptability.

Angstrom-confined Electrochemical Synthesis of Sub-unit Cell non van der Waals 2D Metal Oxides.

Bottom-up electrochemical synthesis of atomically thin materials is desirable yet challenging, especially for non-van der Waals (vdW) materials. Thicknesses below few nm have not been reported yet, posing the question how thin can non-vdW materials be electrochemically synthesized? This is important as materials with (sub-) unit cell thickness often show remarkably different properties compared to their bulk form or thin films of several nm thickness. Here, we introduce a straightforward electrochemical method utilizing the angstrom-confinement of laminar reduced graphene oxide (rGO) nanochannels to obtain a centimeter-scale network of atomically thin (< 4.3 Å) 2D-transition metal oxides (2D-TMO). The angstrom-confinement provides a thickness limitation, forcing sub-unit cell growth of 2D-TMO with oxygen and metal vacancies. We showcase that Cr2 O3 , a material without significant catalytic activity for OER in bulk form, can be activated as a high-performing catalyst if synthesized in the 2D sub-unit cell form. Our method displays the high activity of sub-unit cell form while retaining the stability of bulk form, promising to yield unexplored fundamental science and applications. We show that while retaining the advantages of bottom-up electrochemical synthesis like simplicity, high yield, and mild conditions, the thickness of TMO can be limited to sub-unit cell dimensions. This article is protected by copyright. All rights reserved.

Diversity-Oriented Synthesis of Benzo[f][1,4]oxazepine-, 2H-Chromene-, and 1,2-Dihydroquinoline-Fused Polycyclic Nitrogen Heterocycles under Microwave-Assisted Conditions.

An efficient, diversity-oriented synthesis of oxazepino[5,4-b]quinazolin-9-ones, 6H-chromeno[4,3-b]quinolines, and dibenzo[b,h][1,6]naphthyridines was established involving a substrate-based approach under microwave-assisted and conventional heating conditions in high yields (up to 88%). The CuBr2-catalyzed, chemoselective cascade annulation of O-propargylated 2-hydroxybenzaldehydes and 2-aminobenzamides delivered oxazepino[5,4-b]quinazolin-9-ones involving a 6-exo-trig cyclization-air oxidation-1,3-proton shift-7-exo-dig cyclization sequence. This one-pot process showed excellent atom economy (-H2O) and constructed two new heterocyclic rings (six- and seven-membered) and three new C-N bonds in a single synthetic operation. On the other side of diversification, the reaction between O/N-propargylated 2-hydroxy/aminobenzaldehydes and 2-aminobenzyl alcohols delivered 6H-chromeno[4,3-b]quinolines and dibenzo[b,h][1,6]naphthyridines involving sequential imine formation-[4 + 2] hetero-Diels-Alder reaction-aromatization steps. The influence of microwave assistance was superior to conventional heating, where the reactions were clean, rapid, and completed in 15 min, and the conventional heating required a longer reaction time at a relatively elevated temperature.