Facile Protocol Research Articles

Externally modified Bi12SiO20 with BiOI: n-p heterojunctions for effectually photocatalytic degradation of bisphenol A

The effectual removal of bisphenol A (BPA) molecules is of great significance considering the hazards to the environment and human health. For such, externally BiOI-decorated Bi12SiO20 (BSI) composites were successfully fabricated via a facile post-synthesis protocol and systematically characterized by various analytical techniques. Both expected components were identified and combined tightly in composites to generate n-p heterojunction structures. Under the visible light, these n-p heterojunction composites BSI provided the significantly improved photocatalytic removal abilities of colorless BPA. Particularly, the best candidate BSI-60 owned the largest apparent reaction rate constant (Kapp) 32.72 × 10−3 min−1 that were 48.8 and 2.04 times of those Bi12SiO20 and mixture BSI 60, mainly attributing to the enlarged specific surface area (SBET), strengthened visible light harvesting, and boosted charge carriers separation and further active species generation by heterojunction structures with the suitable phase composition. These composites possessed favorable reusability and structural stability and followed a typical type-II mechanism in the light of entrapping experimental and analytical results. This study may provide a research guidance for the creation of Bi12SiO20-based composites for effectual BPA removal through photocatalytic processes under visible light.

Catalyst‐free oxidative [3+2]‐annulation of (2‐nitroethene‐1,1‐diyl)bis(methylsulfane) and pyridinium ylides: Efficient synthesis of (methylsulfanyl)indolizines heterocycles

AbstractA facile and efficient protocol has been developed for the synthesis of (methylsulfanyl)indolizine derivatives via oxidative [3+2]‐annulation of bis(methylthio)‐2‐nitroethylen(BMTNE) and pyridinium ylides under K2CO3. The target products could be obtained in moderate to good yields.

Insights into Stereoselectivity Switch in Michael Addition-Initiated Tandem Mannich Cyclizations and Their Extension from Enamines to Vinyl Ethers.

Both cis- and trans- tetracyclic spiroindolines are the core of many important biologically active indole alkaloids, but the divergent synthesis of these important motifs is largely hampered by the limited stereoselectivity control. A facile stereoinversion protocol is reported here in Michael addition-initiated tandem Mannich cyclizations for constructing tetracyclic spiroindolines, providing an easy access to two diastereoisomeric cores of monoterpene indole alkaloids with high selectivity. The mechanistic studies including in situ NMR experiments, control experiments, and DFT calculations reveal that the reaction undergoes a unique retro-Mannich/re-Mannich rearrangement including a C-C bond cleavage that is very rare for a saturated six-membered carbocycle. Insights into the stereoinversion process have been uncovered, and the major effects were determined to be the electronic properties of N-protecting groups of the indole with the aid of Lewis acid catalysts. By understanding these insights, the stereoselectivity switching strategy is also smoothly applied from enamine substrates to vinyl ether substrates, which are enriched greatly for the divergent synthesis and stereocontrol of monoterpene indole alkaloids. The current reaction also proves to be very practical and was successfully applied to the gram-scale total synthesis of strychnine and deethylibophyllidine in short routes.

Anti-tumoral Titanium(IV) Complexes Stabilized with Phenolato Ligands and Structure-Activity Relationship.

Titanocene dichloride and budotitane have opened a new chapter in medicinal chemistry of titanium(IV) complexes being novel non-platinum antitumor metallic agents. Numerous efforts have led to the discovery of the diamino bis-phenolato titanium(IV) complexes. Among which, the [ONNO] and [ONON] type ligands namely Salan, Salen and Salalen coordinated titanium(IV) alkoxyl complexes have demonstrated significantly enhanced aqueous stability, their in vitro and in vivo antitumor efficacy, mechanism of action, structure-activity relationships and combined tumor therapy have been intensively investigated. Replacement of the labile alkoxyls with a second chelator resulted in structural rigid titanium(IV) complexes, which showed exceedingly good aqueous stability and potent antitumor activity both in vitro and in vivo. The unique ligand system successfully allowed the access of isotopic [45Ti]Titanium(IV) complexes, post-synthetic modification, facile synthetic protocols and antitumor congeneric zirconium(IV) and hafnium(IV) complexes. This review presents recent research progress in the field of antitumor group 4 metal complexes stabilized with phenolato ligands; especially their structure-activity relationships are summarized.

One-Step Synthesis of Structurally Stable CO2-Philic Membranes with Ultra-High PEO Loading for Enhanced Carbon Capture

Membrane technology has been considered a promising strategy for carbon capture to mitigate the effects of increasing atmospheric CO 2 levels because CO 2 -philic membranes have demonstrated significant application potential, especially, for CO 2 /light gas separation. In this regard, poly(ethylene oxide) (PEO), which is a representative CO 2 -philic material, has attracted extensive research attention owing to its specific dipole–quadrupole interaction with CO 2 . Herein, we report a facile one-step synthesis protocol via the in situ polymerization of highly flexible polyethylene glycol to overcome the limitations of PEO, including high crystallinity and poor mechanical strength. The robust structure derived from intricate entanglements between short PEO chains and the polymer matrix enables an extremely high loading of linear polyethylene glycol (up to 90 wt%). Consequently, the separation performance easily surpasses the upper-bound limit. Moreover, the high structural stability allows for the concurrent increase of CO 2 permeability and CO 2 /light gas selectivity at high feed pressure (up to 20 bar). This study provides a promising strategy to simultaneously improve the toughness and gas separation properties of all-polymeric membranes, demonstrating significant potential for industrial carbon capture and gas purification.

Necessary Products for the Prevention and Treatment of Pressure Injuries: Lessons Learned That Translate Beyond the COVID-19 Pandemic.

To identify the challenges encountered in obtaining the required support surfaces and products to meet pressure injury (PrI) prevention and treatment needs during COVID-19. The authors used SurveyMonkey to gather data on healthcare perceptions and the challenges experienced regarding specific product categories deemed necessary for PrI prevention and treatment in US acute care settings during the pandemic. They created three anonymous surveys for the target populations of supply chain personnel and healthcare workers. The surveys addressed healthcare workers' perceptions, product requests, and the ability to fulfill product requests and meet facility protocols without substitution in the categories of support surfaces and skin and wound care supplies. Respondents answered one of the three surveys for a total sample of 174 respondents. Despite specific instructions, nurses responded to the surveys designed for supply chain personnel. Their responses and comments were interesting and capture their perspectives and insights. Three themes emerged from the responses and general comments: (1) expectations differed between supply chain staff and nurses for what was required for PrI prevention and treatment; (2) inappropriate substitution with or without proper staff education occurred; and (3) preparedness. It is important to identify experiences and challenges in the acquisition and availability of appropriate equipment and products for PrI prevention and treatment. To foster ideal PrI prevention and treatment outcomes, a proactive approach is required to face daily issues or the next crisis.

Content Analysis of Water Birth Policies With Implications for Practice and Research

ObjectiveTo identify areas of agreement and variation in clinical guidance documents (protocols, policies, or guidelines) that direct water birth care. DesignQualitative descriptive. SettingThe clinical guidance documents studied covered water birth in home and hospital settings. SampleThe sample included 22 water birth guidance documents in English from six countries. The documents were obtained by request and resulting snowball sampling. MeasurementsThe framework method was adapted as an analytic tool, and a structured matrix output was used to organize and support the method of qualitative content analysis using a general inductive approach. Areas of general agreement and variations in practice guidelines for water birth were identified. ResultsCriteria for a term, singleton, and cephalic presentation with reassuring maternal and fetal status were the most consistent for inclusion. The reliance on “low-risk” status was strongly present but without a uniform definition. A history of previous cesarean birth, body mass index, use of opioid pain medication, adequate labor progress, and vaginal bleeding were found to vary in directed care, and scarce supporting evidence was offered. Meconium-stained fluid variably excluded water birth in most documents, but this was not supported by evidence. The inconsistent findings from this study are cohesive in the evidence they provide for needed research in areas that affect access to water birth. The findings also provide nurses and birth providers with evidence-based guidelines for water birth care. ConclusionThere was variation across guidance documents, demonstrating that water immersion is a flexible intervention that can be implemented in different settings and locations while following individual facility protocols for processes for care. An identified area of concern comes from examples of overly restrictive policies for water birth based on opinion or perceived risk rather than evidence from research.

Synthesis of N-aryl derived formamides using triflic anhydride

A facile and convenient one-pot protocol for the N-formylation of aryl amines has been furnished using Tf2O. This approach involves N-formylation of anilines and its derivatives employing formic acid as a formyl source and triflic anhydride (Tf2O) as an activator as the key step. This work highlights the ability of Tf2O as an activating agent, includes operational simplicity, easy applicability to gram-scale preparation and to afford the N-formyl aryl amines in moderate to good yields.

A Facile synthesis of Biaryl ketones in recyclable system: Triazenes as new coupling partners in the carbonylative Suzuki and Hiyama cross‐coupling reactions using NFSac as CO source

AbstractPalladium‐catalyzed carbonylation reactions aid as potent tools for the insertion of carbonyl unit(s) in a wide array of molecules possessing vast number of applications in multiple domains. An efficient and facile protocol has been reported for the carbonylative Suzuki (CO−S) and carbonylative Hiyama (CO−H) coupling of aryl triazenes using phenyl boronic acid and triethoxy(phenyl)silane respectively via a Pd‐catalysis in combination with Ionic liquids (ILs). Four different ILs have been employed as solvent/reagent/promotor(s) to afford the targeted products in reasonably good yields. As per the predictive mechanism, an in situ generated N‐Heterocarbene‐Ionicliquid‐Palladium (NHC‐IL‐Pd) species serve as a regenerative catalyst while the N‐formyl saccharin (NFSac), a non‐hazardous and commercially available crystalline compound was used as carbon monoxide (CO) surrogate playing important roles to accomplish the desired products in good yields.

N‐Chlorosuccinimide Mediated Direct C−H Thiocyanation of 1‐Aryl‐5‐pyrazolones at Room Temperature

AbstractA facile synthetic protocol has been established for the N‐chlorosuccinimide (NCS) promoted direct C−H thiocyanation of 1‐aryl‐5‐pyrazolones via in situ‐generated electrophilic thiocyanating agent at room temperature. The current protocol features easy performance, mild conditions and short reaction time using readily available starting materials. The DFT studies suggested that ionic process is likely to be involved in this transformation yielding the targeted product with the most stable enaminone form as the favoured tautomer.

An Expedient Three-component Synthesis of Novel Pyrido-pyrimidine Derivatives: Antimicrobial Activity, Molecular Docking, and ADME Studies

A facile and efficient protocol for one-pot three-component synthesis of a series of novel 4-substituted-2-thioxo-3,4-dihydro-1H-pyrido[1,2-a]pyrimido[4,5-d]pyrimidin-5(2H)-one derivatives has been developed. Compounds were synthesized by the reaction of 2H-pyrido[1,2-a]pyrimidine-2,4(3H)-dione, various aromatic aldehydes, and thiourea using Iodine as catalyst in acidic medium. The synthesized compounds obtained in good to excellent yields (52–83%) with improved reaction time and chloro substituent at four-position yielded the product in excellent quantity (83%). The synthesized compounds have been characterized by 1H, and 13C NMR, IR, and mass spectral analysis, and screened for their in vitro antibacterial activity against Bacillus subtilis, Salmonella typhemurium, Escherichia. coli, and Staphylococcus aureus using disk diffusion method. Biological screening revealed that the newly synthesized compounds exhibit interesting activities against several bacterial strains. Among all the synthesized compounds, the in vitro antibacterial activity displayed by compound 6j was highest against S. typhemurium with ZOI 23.5. mm (MIC = 3.125 µg/mL). Docking studies further supported the findings, and provided for the basis of linkages in terms of conventional hydrogen bonds, and pi- bonding patterns. In nutshell, the present study thus paved the way for developing lead compounds which could be potentially used as an efficient antibacterial drug in humans after appropriate animal, and clinical trials.

Macrocyclic β‐Sheets Stabilized by Hydrogen Bond Surrogates

AbstractMimics of protein secondary and tertiary structure offer rationally‐designed inhibitors of biomolecular interactions. β‐Sheet mimics have a storied history in bioorganic chemistry and are typically designed with synthetic or natural turn segments. We hypothesized that replacement of terminal inter‐β‐strand hydrogen bonds with hydrogen bond surrogates (HBS) may lead to conformationally‐defined macrocyclic β‐sheets without the requirement for natural or synthetic β‐turns, thereby providing a minimal mimic of a protein β‐sheet. To access turn‐less antiparallel β‐sheet mimics, we developed a facile solid phase synthesis protocol. We surveyed a dataset of protein β‐sheets for naturally observed interstrand side chain interactions. This bioinformatics survey highlighted an over‐abundance of aromatic–aromatic, cation‐π and ionic interactions in β‐sheets. In correspondence with natural β‐sheets, we find that minimal HBS mimics show robust β‐sheet formation when specific amino acid residue pairings are incorporated. In isolated β‐sheets, aromatic interactions endow superior conformational stability over ionic or cation‐π interactions. Circular dichroism and NMR spectroscopies, along with high‐resolution X‐ray crystallography, support our design principles.

Macrocyclic β-Sheets Stabilized by Hydrogen Bond Surrogates.

Mimics of protein secondary and tertiary structure offer rationally-designed inhibitors of biomolecular interactions. β-Sheet mimics have a storied history in bioorganic chemistry and are typically designed with synthetic or natural turn segments. We hypothesized that replacement of terminal inter-β-strand hydrogen bonds with hydrogen bond surrogates (HBS) may lead to conformationally-defined macrocyclic β-sheets without the requirement for natural or synthetic β-turns, thereby providing a minimal mimic of a protein β-sheet. To access turn-less antiparallel β-sheet mimics, we developed a facile solid phase synthesis protocol. We surveyed a dataset of protein β-sheets for naturally observed interstrand side chain interactions. This bioinformatics survey highlighted an over-abundance of aromatic-aromatic, cation-π and ionic interactions in β-sheets. In correspondence with natural β-sheets, we find that minimal HBS mimics show robust β-sheet formation when specific amino acid residue pairings are incorporated. In isolated β-sheets, aromatic interactions endow superior conformational stability over ionic or cation-π interactions. Circular dichroism and NMR spectroscopies, along with high-resolution X-ray crystallography, support our design principles.

Encouraging Improvements to Opioid and Substance Use Disorder Care Quality in Nursing Homes

Encouraging Improvements to Opioid and Substance Use Disorder Care Quality in Nursing Homes

Digital Microfluidics and Magnetic Bead-Based Intact Proteoform Elution for Quantitative Top-down Nanoproteomics of Single C. elegans Nematodes.

While most nanoproteomics approaches for the analysis of low-input samples are based on bottom-up proteomics workflows, top-down approaches enabling proteoform characterization are still underrepresented. Using mammalian cell proteomes, we established a facile one-pot sample preparation protocol based on protein aggregation on magnetic beads and intact proteoform elution using 40 % formic acid. Performed on a digital microfluidics device, the workflow enabled sensitive analyses of single Caenorhabditis elegans nematodes, thereby increasing the number of proteoform identifications compared to in-tube sample preparation by 46 %. Label-free quantification of single nematodes grown under different conditions allowed to identify changes in the abundance of proteoforms not distinguishable by bottom-up proteomics. The presented workflow will facilitate proteoform-directed analysis on samples of limited availability.

Elution von intakten Proteoformen von magnetischen Partikeln kombiniert mit digitaler Mikrofluidik für die quantitative Top‐down‐Nanoproteomik von einzelnen C. elegans‐Nematoden

AbstractWährend die meisten Ansätze zur Analyse von geringen Probemengen durch Nanoproteomik auf der bottom‐up‐Strategie basieren, sind top‐down‐Ansätze zur Charakterisierung von Proteoformen nach wie vor unterrepräsentiert. An Proteomen von Säugerzellen haben wir eine einfache Probenvorbereitungsmethode etabliert, welche auf Proteinaggregation an magnetischen Partikeln und anschließender Elution intakter Proteoformen durch 40 %ige Ameisensäure basiert. Die Implementierung der Methode auf einer Plattform für digitale Mikrofluidik ermöglichte die sensitive Analyse von einzelnen Individuen des Nematoden Caenorhabditis elegans. Die Anzahl identifizierter Proteoformen konnte dabei im Vergleich zu herkömmlicher Probenvorbereitung in einem Reaktionsgefäß um 46 % erhöht werden. Ferner erlaubte die markierungsfreie (label‐free) Quantifizierung von Proteomen einzelner Nematoden, welche unter verschiedenen Bedingungen kultiviert wurden, Änderungen der Abundanz von Proteoformen zu erkennen, welche in bottom‐up‐Experimenten nicht festgestellt wurden. Die hier präsentierte Methode wird die Proteoform‐zentrische Analytik in Proben mit limitierter Verfügbarkeit vereinfachen.

0108 Sleep Health of Adolescents in the Department of Juvenile Justice: A Qualitative Analysis of Night Staff Interviews

Abstract Introduction Limited research exists regarding the sleep environment and sleep health of youth in juvenile justice facilities. We examined the perspectives of facility night staff on the sleep-living environment and conditions of detained youth using semi-structured interviews. Methods In collaboration with Maryland’s Department of Juvenile Services (DJS) we conducted virtual semi-structured interviews (45 minutes) with superintendents, medical staff, and night staff at all state facilities. We present the data reported by night staff (n=10) here, each representing a different facility. Interview questions focused on facility structure, protocols, and youth healthcare. Inductive qualitative analyses examined high frequency themes with the aim of understanding the sleep environment, sleep patterns, and overall youth wellbeing. After transcription of each interview, coder 1 examined each transcript to identify high frequency themes; coder 2 reviewed these first codes. Few disagreements occurred; in those cases, a third coder helped reach consensus. Theme frequency is expressed as a percentage of the total number of transcriptions (e.g., 4 interviews out of 10=40%). Results Major themes reported by night staff include environmental disruptions, ability to personalize sleep areas, youth well-being, and sleep challenges. Environmental disruptions included moderate noise levels (40%); youth temperature complaints (50%); and youth lighting complaints (60%). More specifically, 50% reported youth reported night lighting complaints (including blue light) within the dorms. While 40% described room personalization is allowed, 40% stated it is also limited. For instance, while youth are allowed to display family pictures, they are not allowed to display any gang-related material as it could cause altercations between youth. Complaints of trouble sleeping is addressed in 50% of facilities by utilizing a weeklong sleeping log (e.g., staff report number of times youth are awake during the night during their safety checks). Seventy percent of staff reported that work affects their sleep and psychological wellbeing and 60% shared that they sleep 3 - 6 hours/night. Conclusion Assessment and modifications of the sleep-living environment in juvenile justice facilities are needed. Ongoing countermeasures in the Maryland system include noise buffering panels, light modifications, and sleep-health staff trainings. Support (if any) Kolvenbach grant, Loyola University Maryland and Maryland Department of Juvenile Services’ supportive collaboration.

Molecular Precursor-Driven Synthesis of Copper Telluride Nanostructures for LIB Anode Application.

Copper tellurides have garnered substantial interest for their applicability as an electrocatalyst for water splitting, battery anodes and photodetectors, etc. Moreover, synthesis of phase pure metal tellurides using the multi-source precursor method is challenging. Therefore, a facile synthesis protocol for copper tellurides is anticipated. The current study involves a simplistic single source molecular precursor pathway for the synthesis of orthorhombic-Cu2.86Te2 nano blocks and -Cu31Te24 faceted nanocrystals employing the [Cu{TeC5H3(Me-5)N}]4 cluster in thermolysis and pyrolysis, respectively. The pristine nanostructures were carefully characterized by powder X-ray diffraction, energy-dispersive X-ray spectroscopy, electron microscopic techniques (scanning electron microscopy and transmission electron microscopy), and diffuse reflectance spectroscopy to know the crystal structure, phase purity, elemental composition, distribution of elements, morphology, and optical band gap. These measurements suggests that the reaction conditions fetch nanostructures of different sizes, crystal structures, morphologies, and band gaps. As prepared nanostructures were evaluated for lithium-ion batteries (LIBs) anode material. The cells fabricated with orthorhombic Cu2.86Te2 and orthorhombic Cu31Te24 nanostructures deliver capacities of 68 and 118 mA h/g after 100 cycles. The LIB anode made up of Cu31Te24 faceted nanocrystals exhibited good cyclability and mechanical stability.

Green synthesis of bismuth nanoparticles using green coffee beans extract

A green synthetic process based on plant sources could be an alternative option to conventional chemical one to synthesize nanostructured bismuth. This study explored a facile and green synthetic protocol for synthesizing bismuth nanoparticles (BiNPs) in an aqueous solution employing green coffee bean extract as a key reducing and capping agent. Several techniques, including X-ray diffraction, electron microscopy, energy dispersive X-ray and Fourier-transform infrared spectroscopy, and thermogravimetric analysis, have been used to characterize the resultant product. The outcomes show that crystalline BiNPs are successfully produced using the green synthesis method based on plant sources. The obtained BiNPs have a spherical shape, a diameter ranges of 20 to 40 nm, and are stabilized by phytochemicals. The purpose of the current study is to ascertain the potential impact of plant sources on the environmentally friendly synthesis of BiNPs.

Synthesis of 4-Aryl-1,3,4-benzotriazepinones from Isatoic Anhydrides and Hydrazonyl Chlorides

An efficient synthesis of 4-aryl-1,3,4-benzotriazepinones from readily available isatoic anhydrides and hydrazonyl chlorides was developed. In this facile protocol, a series of functionalized 1,3,4-benzotriazepinones were conveniently obtained with broad substrate scope and excellent functional group tolerance.