Mechanochemical synthesis of hyper-crosslinked polymers: influences on their pore structure and adsorption behaviour for organic vapors

• Sven Grätz,
• Sebastian Zink,
• Hanna Kraffczyk,
• Marcus Rose and
• Lars Borchardt

Beilstein J. Org. Chem. 2019, 15, 1154–1161, doi:10.3762/bjoc.15.112

• protocol the polymer obtained through this mechanochemical route is also amorphous as visualized by the XRD (X-ray diffraction) patters recorded (Supporting Information File 1, Figure S1) [43]. Furthermore, NG-HCP similarly shows a high thermal stability with a decomposition onset in air (Supporting

Fabrication, characterization and adsorption properties of cucurbit[7]uril-functionalized polycaprolactone electrospun nanofibrous membranes

• Changzhong Chen,
• Fengbo Liu,
• Xiongzhi Zhang,
• Zhiyong Zhao and
• Simin Liu

Beilstein J. Org. Chem. 2019, 15, 992–999, doi:10.3762/bjoc.15.97

• , Xiangnan University, Chenzhou 423000, China 10.3762/bjoc.15.97 Abstract The fabrication of electrospun nanofibers comprising cucurbit[7]uril (CB[7]) and poly(ε-caprolactone) (PCL) is reported. Various techniques such as SEM, FTIR, XRD, DSC and TG were utilized to characterize the morphology, composition

• dispersion and crystallization of CB[7] and PCL in the composite nanofibers, XRD patterns of neat PCL nanofibers and all PCL/CB[7] nanofibers were recorded (Figure 2). PCL is a semi-crystalline polymer, and neat PCL nanofibers elicit two strong and sharp characteristic diffraction peaks at 2θ = 22° and 2θ

• = 24.5° which correspond to (110) and (200) reflections, respectively [12][15][17]. On the other hand, there are two wider diffraction peaks at 2θ = 13° and 2θ = 21.2° in the XRD curve of CB[7] powders. From the XRD curves of the PCL/CB[7] nanofibers, the sharp diffraction peaks of PCL and wide

Fabrication of supramolecular cyclodextrin–fullerene nonwovens by electrospinning

• Hiroaki Yoshida,
• Ken Kikuta and
• Toshiyuki Kida

Beilstein J. Org. Chem. 2019, 15, 89–95, doi:10.3762/bjoc.15.10

• structurally amorphous fiber materials consistently [9][11]. In this work, we expected that the incorporation of C60 into γ-CD nanofibers helps with the regular arrangement of γ-CD molecules, but γ-CD–C60 microfiber materials do not also show a specific XRD pattern (Figure S8 in Supporting Information File 1

• Information Supporting Information File 2: UV–vis and viscosity measurements of the spinning solutions, electrospinning at various parameters, and XRD patterns of the prepared nonwovens. Acknowledgements This research was financially supported by a research fund from Kondo Memorial Foundation and a Grant in

MoO₃ on zeolites MCM-22, MCM-56 and 2D-MFI as catalysts for 1-octene metathesis

• Hynek Balcar,
• Martin Kubů,
• Naděžda Žilková and
• Mariya Shamzhy

Beilstein J. Org. Chem. 2018, 14, 2931–2939, doi:10.3762/bjoc.14.272

• –Grubbs type hybrid catalysts active in metathesis of long-chain unsaturated esters [24]. Results and Discussion Catalyst preparation and characterization XRD patterns and texture properties (Table 1, Figure 1 A,B,C,D) of prepared MCM-22, MCM-56 and 2D-MFI zeolites proved a high quality of these supports

• already observed earlier [9][10][24]. For x MoO3/MCM-22(28), XRD patterns of catalysts are similar to those of their parents approximately up to x = 6 wt % of Mo (0.9 Mo atoms per nm2). At higher Mo concentrations signals of crystalline MoO3 appeared (marked with * in Figure 1 A,B,D). It suggests 6 wt

• , catalysts with 6 wt % (and lower) content of Mo did not exhibit any MoO3 signals. It is consistent with the previous observation that MoO2(acac)2 provided better catalyst than MoO3 [9]. XRD patterns of 6MoO3/MCM-56(13) and 6MoO3/2D-MFI(26) indicated also a good MoO3 spreading, contrary to 6MoO3/HZSM-5(25

An overview on recent advances in the synthesis of sulfonated organic materials, sulfonated silica materials, and sulfonated carbon materials and their catalytic applications in chemical processes

• Hashem Sharghi,
• Pezhman Shiri and
• Mahdi Aberi

Beilstein J. Org. Chem. 2018, 14, 2745–2770, doi:10.3762/bjoc.14.253

• minutes at 70 °C, a dark green soiled salt was obtained in 98% yield. The catalyst was characterized by different analyses. The FE-SEM images exhibited that the particles of the catalyst are in nano size. According to XRD pattern, the crystallite size is at about 13.7 nm. The IR spectrum confirmed the

Transition metal-free oxidative and deoxygenative C–H/C–Li cross-couplings of 2H-imidazole 1-oxides with carboranyl lithium as an efficient synthetic approach to azaheterocyclic carboranes

• Lidia A. Smyshliaeva,
• Mikhail V. Varaksin,
• Pavel A. Slepukhin,
• Oleg N. Chupakhin and
• Valery N. Charushin

Beilstein J. Org. Chem. 2018, 14, 2618–2626, doi:10.3762/bjoc.14.240

• be attributed to C-2 of the imidazole ring. The structure of imidazolyl carborane 5d has also been proved by the X-ray analysis (Figure 3). The single crystals were obtained by slow evaporation of imidazolyl carborane 5d from a mixture of CH2Cl2/heptane, 8:2. According to the XRD data, two

Calixazulenes: azulene-based calixarene analogues – an overview and recent supramolecular complexation studies

• Paris E. Georghiou,
• Shofiur Rahman,
• Abdullah Alodhayb,
• Hidetaka Nishimura,
• Jaehyun Lee,
• Atsushi Wakamiya and
• Lawrence T. Scott

Beilstein J. Org. Chem. 2018, 14, 2488–2494, doi:10.3762/bjoc.14.225

• solvents prevented a fuller examination of its potential supramolecular properties with fullerenes, a topic of particular interest to us [18]. Therefore, the solid state supramolecular complexation properties of 5 were experimentally studied using solid state NMR and XRD experiments, and also theoretically

Bioinspired cobalt cubanes with tunable redox potentials for photocatalytic water oxidation and CO₂ reduction

• Zhishan Luo,
• Yidong Hou,
• Jinshui Zhang,
• Sibo Wang and
• Xinchen Wang

Beilstein J. Org. Chem. 2018, 14, 2331–2339, doi:10.3762/bjoc.14.208

• observed at ≈759, ≈692, ≈634 and ≈574 cm−1, corresponding to the “Co4O4” cubane-like core present in the complex [54]. The XRD patterns for 1-R cubanes are shown in Supporting Information File 1, Figure S8. Moreover, as shown in Scheme S1 (Supporting Information File 1), all aqueous solutions of 1-R are

• TECNAIG2F20 instrument. Powder X-ray diffraction (XRD) patterns were collected on Bruker D8 Advance diffractometer with Cu K1 radiation (λ = 1.5406 Å). Photocatalytic test for water oxidation system [69]: Photocatalytic O2 production was carried out in a Pyrex top-irradiation reaction vessel connected to a

Bi-mediated allylation of aldehydes in [bmim][Br]: a mechanistic investigation

• Mrunesh Koli,
• Sucheta Chatterjee,
• Subrata Chattopadhyay and
• Dibakar Goswami

Beilstein J. Org. Chem. 2018, 14, 2198–2203, doi:10.3762/bjoc.14.193

• the powder XRD analysis of the light yellow precipitate. Earlier, it has been reported [38][43] that the organobismuth halide generated in situ may act as a Lewis acid activator for the faster production of linear homoallylic alcohols. In the present case also, such a mechanism cannot be excluded

Revisiting ring-degenerate rearrangements of 1-substituted-4-imino-1,2,3-triazoles

• James T. Fletcher,
• Matthew D. Hanson,
• Joseph A. Christensen and
• Eric M. Villa

Beilstein J. Org. Chem. 2018, 14, 2098–2105, doi:10.3762/bjoc.14.184

• pairings of reactants. Crystals of 2cc’ suitable for XRD analysis were grown from slow evaporation of a methylene chloride solution. As shown in Figure 2, each of the three aromatic rings in this molecule’s fully conjugated π-system adopts a largely coplanar configuration. The dihedral angle between the 1

• Union Road, Cambridge, CB2 1EZ, UK (fax: +44-(0)1223-336033 or e-mail: despoit@ccdc.cam.ac.uk). Supporting Information File 474: Experimental procedures, copies 1H and 13C NMR spectra for all reported compounds, details of XRD analysis and UV–visible spectra for kinetic assays. Acknowledgements This

Graphitic carbon nitride prepared from urea as a photocatalyst for visible-light carbon dioxide reduction with the aid of a mononuclear ruthenium(II) complex

• Kazuhiko Maeda,
• Daehyeon An,
• Ryo Kuriki,
• Daling Lu and
• Osamu Ishitani

Beilstein J. Org. Chem. 2018, 14, 1806–1812, doi:10.3762/bjoc.14.153

• reactions. Results and Discussion Synthesis of g-C3N4 by thermal heating of urea at different temperatures Figure 1 shows XRD patterns of g-C3N4 samples synthesized at different temperatures. Two peaks are observed at 2theta = 13 and 27.4°, which are assigned to an in-planar repeating motif and the stacking

• increasing temperature. This further indicates the production of g-C3N4 at elevated temperatures, consistent with the XRD analysis (Figure 1). The 812 cm−1 peak is attributed to the out-of-plane bending vibration characteristic of heptazine rings. The results of elemental analyses for the as-prepared g-C3N4

• ). MeCN was distilled over P2O5 twice, and then distilled over CaH2 prior to use. TEOA was distilled under reduced pressure (<1 Torr). The distilled DMA and TEOA were kept under Ar prior to use. Characterization The prepared materials were characterized by X-ray diffraction (XRD) (MiniFlex600, Rigaku; Cu

Cobalt–metalloid alloys for electrochemical oxidation of 5-hydroxymethylfurfural as an alternative anode reaction in lieu of oxygen evolution during water splitting

• Jonas Weidner,
• Stefan Barwe,
• Kirill Sliozberg,
• Stefan Piontek,
• Justus Masa,
• Ulf-Peter Apfel and
• Wolfgang Schuhmann

Beilstein J. Org. Chem. 2018, 14, 1436–1445, doi:10.3762/bjoc.14.121

• -temperature synthesis from the elements and was obtained by salt metathesis from Mg2Si and CoCl2 at 400 °C under inert conditions. Characterization of the materials was performed using powder XRD (Figure 1). For Co2Si, the observed reflexes correlate well with those observed for PXRD patterns generated from

• dilution with 990 μL water. Physical characterization X-ray diffractometry XRD data were obtained using a Panalytical X'PERT Pro MPD X-ray diffractometer with a Cu Kα radiation source (λ = 1.5418 Å) in the 2θ = 20–80° range. Scanning electron microscopy SEM images were taken using a Quanta ED FEG scanning

• electron microscope (FEI). The SEM was operated at 20 kV. XRD patterns of Co2Si, CoTe, CoAs. Cobalt is indicated by (+) and signals corresponding to the desired materials are indicated by (*). Linear sweep voltammograms of CoP, CoB, CoTe, Co2Si, CoAs modified and blank Ni RDEs for the OER (a) and the HMF

Mechanochemistry of nucleosides, nucleotides and related materials

• Olga Eguaogie,
• Joseph S. Vyle,
• Patrick F. Conlon,
• Manuela A. Gîlea and
• Yipei Liang

Beilstein J. Org. Chem. 2018, 14, 955–970, doi:10.3762/bjoc.14.81

• using mechanochemistry [94] and Rajamohan and co-workers described using a mortar and pestle to effect LAG of β-cyclodextrin with either inosine [95] or cytidine [96] in the presence of water. Weak complex formation was inferred by powder XRD for cytidine. Conclusion Access to reliable and reproducible

Heterogeneous Pd catalysts as emulsifiers in Pickering emulsions for integrated multistep synthesis in flow chemistry

• Katharina Hiebler,
• Georg J. Lichtenegger,
• Manuel C. Maier,
• Eun Sung Park,
• Renie Gonzales-Groom,
• Bernard P. Binks and
• Heidrun Gruber-Woelfler

Beilstein J. Org. Chem. 2018, 14, 648–658, doi:10.3762/bjoc.14.52

• analysed using different state-of-the-art methods. Details of the characterisation were published recently [37]. Here, only the most important characteristics are summarised. The obtained X-ray diffraction (XRD) profiles proved the nanocrystallinity of the catalyst particles, which either show single phase

• cubic, tetragonal or a more amorphous cubic/tetragonal mixed phase structure depending on the content of Sn. As far as palladium substitution in the lattice is concerned, XRD and X-ray photoelectron spectroscopy (XPS) analysis approved the predominant cationic nature of incorporated palladium (Pd2+) and

Solid-state studies and antioxidant properties of the γ-cyclodextrin·fisetin inclusion compound

• Joana M. Pais,
• Maria João Barroca,
• Maria Paula M. Marques,
• Filipe A. Almeida Paz and
• Susana S. Braga

Beilstein J. Org. Chem. 2017, 13, 2138–2145, doi:10.3762/bjoc.13.212

• XRD data were collected at ambient temperature on an X’Pert MPD Philips diffractometer (Cu Kα1 = 1.540598 Å) with a curved graphite monochromator, equipped with a X’Celerator detector, operating in a flat Bragg–Brentano configuration (40 kV, 50 mA). Data was collected with steps of 0.04° in a

Mechanochemical Knoevenagel condensation investigated in situ

• Sebastian Haferkamp,
• Franziska Fischer,
• Werner Kraus and
• Franziska Emmerling

Beilstein J. Org. Chem. 2017, 13, 2010–2014, doi:10.3762/bjoc.13.197

• excitation wavelength was 785 nm. A typical measurement consists of five accumulated recordings for 5 s. A new measurement was started every 30 s. Single crystal X-ray diffraction: Single crystal XRD measurements were performed on a D8 Venture diffractometer (Bruker AXS, Germany) using Mo Kα radiation (λ

New bio-nanocomposites based on iron oxides and polysaccharides applied to oxidation and alkylation reactions

• Daily Rodríguez-Padrón,
• Alina M. Balu,
• Antonio A. Romero and
• Rafael Luque

Beilstein J. Org. Chem. 2017, 13, 1982–1993, doi:10.3762/bjoc.13.194

• assessed in the alkylation reaction of toluene with benzyl chloride and the selective oxidation of benzyl alcohol to benzaldehyde. X-ray diffraction The structure and arrangement of the synthesized materials were analyzed by X-ray diffraction. The XRD pattern of the Fe2O3-PS4 nanomaterial exhibited a

• of the magnetic material showed a mixture of maghemite and hematite phases. In this case, a similar XRD pattern could be in principle associated to magnetite (Fe3O4) over the maghemite phase, since these two phases are difficult to clearly distinguish by XRD analysis. However, the absence of Fe2

• (Supporting Information File 1, Figure S1C). X-ray photoelectron spectroscopy X-ray photoelectron spectroscopy (XPS) measurements were consistent with XRD data, where the main peaks were found to correspond to Fe2O3 species. In the three nanocomposites, the presence of Fe3+ species could be also inferred from

Ni nanoparticles on RGO as reusable heterogeneous catalyst: effect of Ni particle size and intermediate composite structures in C–S cross-coupling reaction

• Debasish Sengupta,
• Koushik Bhowmik,
• Goutam De and
• Basudeb Basu

Beilstein J. Org. Chem. 2017, 13, 1796–1806, doi:10.3762/bjoc.13.174

• materials were well characterized by powder XRD, TEM, TGA and XPS studies. The preparation and characterization of the nanocomposites were described in detail in our previous publications [48][49]. Usually, bare Ni NPs are unstable and likely to undergo aerial oxidation [43]. However, in the Ni/RGO

• times for the same reaction examined consecutively without any significant drop in catalytic activity. Figure 1 shows the results of consecutive recycle runs. Characterization of the recovered catalyst To establish the reaction mechanism, we characterized the recovered catalyst by Raman, XRD, XPS and

• TEM studies. The Raman and XRD results of fresh Ni/RGO-40 were reported in our previous publication [48]. However, for comparison, Raman and XRD of a fresh Ni/RGO-40 sample were again recorded and presented along with that of the recovered sample. The Raman spectrum of the Ni/RGO-40 composite (Figure

Block copolymers from ionic liquids for the preparation of thin carbonaceous shells

• Sadaf Hanif,
• Bernd Oschmann,
• Dmitri Spetter,
• Muhammad Nawaz Tahir,
• Wolfgang Tremel and
• Rudolf Zentel

Beilstein J. Org. Chem. 2017, 13, 1693–1701, doi:10.3762/bjoc.13.163

• higher temperatures (above 700 °C) is not advisable. Due to the use of TiO2, phase transitions of the anatase TiO2 might occur, which leads to a mixture of anatase and rutile TiO2. XRD measurements (Figure 5) show that under the applied conditions, the pyrolyzed nanoparticles still contain TiO2. In

Encaging palladium(0) in layered double hydroxide: A sustainable catalyst for solvent-free and ligand-free Heck reaction in a ball mill

• Wei Shi,
• Jingbo Yu,
• Zhijiang Jiang,
• Qiaoling Shao and
• Weike Su

Beilstein J. Org. Chem. 2017, 13, 1661–1668, doi:10.3762/bjoc.13.160

• milling (HSBM) conditions at room temperature. The effects of milling-ball size, milling-ball filling degree, reaction time, rotation speed and grinding auxiliary category, which would influence the yields of mechanochemical Heck reactions, were investigated in detail. The characterization results of XRD

• prepared materials We initially prepared the Pd/MgAl-LDHs catalyst as described in the Experimental section (see Supporting Information File 1). Figure 1 shows the powder XRD patterns of MgAl-LDHs, MgAl-LDHs-PdCl42− and Pd/MgAl-LDHs at 2θ = 5–80°. All samples have diffraction peaks located around 10°, 20

• significant loss in coupling product yields. The XRD patterns for the samples of MgAl-LDHs, MgAl-LDHs-PdCl42− and Pd/MgAl-LDHs. Examination of the milling-ball filling degree (ΦMB) and milling-ball sizes on the yield of 3aa. Reaction conditions: 1a (1.5 mmol), 2a (2.1 mmol), Pd/MgAl-LDHs (2.5 mol %), TBAB

Mechanochemical synthesis of graphene oxide-supported transition metal catalysts for the oxidation of isoeugenol to vanillin

• Ana Franco,
• Sudipta De,
• Alina M. Balu,
• Araceli Garcia and
• Rafael Luque

Beilstein J. Org. Chem. 2017, 13, 1439–1445, doi:10.3762/bjoc.13.141

• were characterized by using several techniques including BET, SEM, TEM, XRD, and IR spectroscopy. N2 adsorption/desorption isotherms of the reduced graphene sample (Figure 1a) can be classified as type IV corresponding to the mesoporous materials. The RGO sample showed a BET surface area of 103 m2 g−1

• diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFT). N2 adsorption measurements were performed at 77 K by using a Micromeritics ASAP 2000 volumetric adsorption analyzer. The samples were degassed

• and f) 1% Co/RGO. Powder XRD patterns of RGO supported Fe and Co NPs. IR spectra of 1% Fe/RGO and 1% Co/RGO catalysts collected by using diffuse reflectance infrared transform spectroscopy (DRIFT) at room temperature. Textural properties of RGO and NPs supported RGO materials. Results for the

Mechanochemistry-assisted synthesis of hierarchical porous carbons applied as supercapacitors

• Desirée Leistenschneider,
• Nicolas Jäckel,
• Felix Hippauf,
• Volker Presser and
• Lars Borchardt

Beilstein J. Org. Chem. 2017, 13, 1332–1341, doi:10.3762/bjoc.13.130

• , resulting in a well-connected pore system of the carbon material (Figure 3A,B). To display the complete removal of the porogenous TiO2, we compared the XRD pattern (Figure 4) of the material at different synthesis steps: after mechanochemical polymerization (Polymer-SF-3), after temperature treatment but

• adjustment using the Scherrer equation. Carbochlorination will remove these nanoparticles, leading to mesopores of comparable size. The XRD pattern of the carbon shows the broad (002) reflection of nanocrystalline carbon, but all signals related to titania have disappeared. This assumption was further

• ) isopropoxide (Polymer-SF-3, orange). SEM (A) and TEM (B) images of the Carb-SF-3 sample. XRD-pattern of the polymeric precursor (Polymer-SF-3, orange), the carbonized composite (Comp-SF-3, black) and the carbon received by chlorine treatment (Carb-SF-3, red). Nitrogen physisorption isotherms for carbon samples

Sugar-based micro/mesoporous hypercross-linked polymers with in situ embedded silver nanoparticles for catalytic reduction

• Qing Yin,
• Qi Chen,
• Li-Can Lu and
• Bao-Hang Han

Beilstein J. Org. Chem. 2017, 13, 1212–1221, doi:10.3762/bjoc.13.120

•  3f). The weight percentage of carbon, oxygen, and silver is 85.33%, 7.21% and 7.46%, respectively. The atomic percentage of carbon, oxygen and silver is 93.18%, 5.91% and 0.91%, respectively. The as-synthesized AgNPs/SugPOP-1 composite was also characterized by X-ray diffraction (XRD) with the

Fluorescent carbon dots from mono- and polysaccharides: synthesis, properties and applications

• Stephen Hill and
• M. Carmen Galan

Beilstein J. Org. Chem. 2017, 13, 675–693, doi:10.3762/bjoc.13.67

• our knowledge, the first reported example involving a carbohydrate moiety (Scheme 1) [18]. The water-soluble nanoparticles exhibited an amorphous core, as deduced by X-ray diffraction (XRD), while Fourier-transformed infrared (FTIR) spectroscopy analysis indicated the presence of a range of oxygen

Correction: Synthesis, dynamic NMR characterization and XRD studies of novel N,N’-substituted piperazines for bioorthogonal labeling

• Constantin Mamat,
• Marc Pretze,
• Matthew Gott and
• Martin Köckerling

Beilstein J. Org. Chem. 2017, 13, 301–302, doi:10.3762/bjoc.13.32