Thermal stability of N-heterocycle-stabilized iodanes – a systematic investigation

• Andreas Boelke,
• Yulia A. Vlasenko,
• Mekhman S. Yusubov,
• Boris J. Nachtsheim and
• Pavel S. Postnikov

Beilstein J. Org. Chem. 2019, 15, 2311–2318, doi:10.3762/bjoc.15.223

• Federation Department of Solid State Engineering, University of Chemistry and Technology, 16628 Prague, Czech Republic 10.3762/bjoc.15.223 Abstract The thermal stability of pseudocyclic and cyclic N-heterocycle-stabilized (hydroxy)aryl- and mesityl(aryl)-λ3-iodanes (NHIs) through thermogravimetric analysis

• high N/C-ratio might result in potential hazardous high energy materials, we herein investigated their thermal stability by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Results and Discussion We started our experiments with the preparation of appropriate λ3-iodanes

• ). Cyclic triazole 17 has a significantly higher Tpeak but also a higher ΔHdec compared to the corresponding pseudocycle 2 (134.5 kJ/mol vs 116.3 kJ/mol). Besides pseudocyclic and cyclic hydroxy(aryl)-λ3-iodanes, mesityl(phenyl)- λ3-iodanes 18–33 were systematically investigated by thermogravimetric

N-doped carbon dots covalently functionalized with pillar[5]arenes for Fe³⁺ sensing

• Jia Gao,
• Ming-Xue Wu,
• Dihua Dai,
• Zhi Cai,
• Yue Wang,
• Wenhui Fang,
• Yan Wang and
• Ying-Wei Yang

Beilstein J. Org. Chem. 2019, 15, 1262–1267, doi:10.3762/bjoc.15.123

• confirming the successful synthesis of CCDs. Thermogravimetric analysis (TGA, Figure 1f) revealed that the weight loss at 200 °C was due to the pyrolysis of the amino and oxygen groups on the surface of CN-dots, and upon reaching the temperature of 500 °C, CN-dots began to decompose and 61 wt % of its weight

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

• . Scanning electron microscopy (SEM/EDX) images were obtained using a Hitachi SU8020 SEM equipped with a secondary electron (SE) detector. Prior to the measurement the samples were prepared on an adhesive carbon pad and sputtered with gold to obtain the necessary electron conductivity. Thermogravimetric

• analysis (TGA) was performed on a Netzsch STA 409 PC/PG system using alumina crucibles under argon stream with the heating rate of 10 K min−1. The vapor sorption experiments were carried out using a Autosorb iQ from Quantachrome equipped with a vapor source and a heated manifold. Before evaporation the

Easy, efficient and versatile one-pot synthesis of Janus-type-substituted fullerenols

• Marius Kunkel and
• Sebastian Polarz

Beilstein J. Org. Chem. 2019, 15, 901–905, doi:10.3762/bjoc.15.87

• formula of the compound is identified by electrospray ionization mass spectrometry (ESIMS). The degree of polyhydroxylation and the number of substituents is determined and confirmed with thermogravimetric analysis (TGA) and the nature of oxygen moieties as well as the substituents attached are evaluated

Application of olefin metathesis in the synthesis of functionalized polyhedral oligomeric silsesquioxanes (POSS) and POSS-containing polymeric materials

• Patrycja Żak and
• Cezary Pietraszuk

Beilstein J. Org. Chem. 2019, 15, 310–332, doi:10.3762/bjoc.15.28

• heptacyclopentylnorbornenylethyloctasilsesquioxane and its copolymerization with cyclooctene [43]. The obtained copolymer was subsequently hydrogenated to afford polyethylene–POSS random copolymer (Scheme 21). Thermogravimetric analysis of the polyethylene–POSS copolymers under air showed a significant improvement of the thermal stability relative

Selective formation of a zwitterion adduct and bicarbonate salt in the efficient CO₂ fixation by N-benzyl cyclic guanidine under dry and wet conditions

• Yoshiaki Yoshida,
• Naoto Aoyagi and
• Takeshi Endo

Beilstein J. Org. Chem. 2018, 14, 2204–2211, doi:10.3762/bjoc.14.194

• spectrometer, at a spinning speed of 10 kHz. Thermogravimetric analysis (TGA) was performed on a Seiko Instrument TG-DTA 6200 using an aluminum pan in the temperature range of 30–350 °C at a heating rate of 5 °C/min under a nitrogen atmosphere (flow rate 200 mL/min). Geometry optimized energy for 1, 2 and 3

Recent advances in phosphorescent platinum complexes for organic light-emitting diodes

• Cristina Cebrián and
• Matteo Mauro

Beilstein J. Org. Chem. 2018, 14, 1459–1481, doi:10.3762/bjoc.14.124

• complexes exhibited high thermal stability since thermogravimetric analysis (TGA) showed a weight loss of only 5% at temperatures in the range 436–463 °C. An intense and structured emission in the green region with λem = 500–507 nm and PLQY = 0.6–0.78 was recorded when the complexes were used as dopant in

Two novel blue phosphorescent host materials containing phenothiazine-5,5-dioxide structure derivatives

• Feng-Ming Xie,
• Qingdong Ou,
• Qiang Zhang,
• Jiang-Kun Zhang,
• Guo-Liang Dai,
• Xin Zhao and
• Huai-Xin Wei

Beilstein J. Org. Chem. 2018, 14, 869–874, doi:10.3762/bjoc.14.73

• injection and transmission [21]. Therefore, we successfully synthesized two novel bipolar host materials with higher triplet energy by choosing suitable donor and acceptor units. Thermal properties The thermal properties of CEPDO and CBPDO were determined by thermogravimetric analysis (TGA) and differential

D–A–D-type orange-light emitting thermally activated delayed fluorescence (TADF) materials based on a fluorenone unit: simulation, photoluminescence and electroluminescence studies

• Lin Gan,
• Xianglong Li,
• Xinyi Cai,
• Kunkun Liu,
• Wei Li and
• Shi-Jian Su

Beilstein J. Org. Chem. 2018, 14, 672–681, doi:10.3762/bjoc.14.55

• efficiency of the OLEDs based on conventional fluorescent materials. Results and Discussion 27DACRFT 1 and 36DACRFT 2 have similar thermal properties according to thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) measurements. They have high decomposition temperatures (Td

An alternative to hydrogenation processes. Electrocatalytic hydrogenation of benzophenone

• Cristina Mozo Mulero,
• Alfonso Sáez,
• Jesús Iniesta and
• Vicente Montiel

Beilstein J. Org. Chem. 2018, 14, 537–546, doi:10.3762/bjoc.14.40

• the Pd nanoparticles. Thermogravimetric analysis (TGA) was performed using a Mettler Toledo model TGA/SDTA851 and /SF/1100 using a heating slope of 10 K min−1 from 298 K to 1023 K under a N2:O2 (4:1) atmosphere. For the characterisation of the Pdx/C/T scanning electron microscopy (SEM) micrographs

• a polymer electrolyte membrane electrochemical reactor (PEMER). Palladium (Pd) nanoparticles were synthesised and supported on a carbonaceous matrix (Pd/C) with a 28 wt % of Pd with respect to carbon material. Pd/C was characterised by transmission electron microscopy (TEM), and thermogravimetric

• analysis (TGA). Cathodes were prepared using Pd electrocatalytic loadings (LPd) of 0.2 and 0.02 mg cm−2. The anode consisted of hydrogen gas diffusion for the electrooxidation of hydrogen gas, and a 117 Nafion exchange membrane acted as a cationic polymer electrolyte membrane. Benzophenone solution was

5-Aminopyrazole as precursor in design and synthesis of fused pyrazoloazines

• Ranjana Aggarwal and
• Suresh Kumar

Beilstein J. Org. Chem. 2018, 14, 203–242, doi:10.3762/bjoc.14.15

• also investigated by techniques like fluorescence spectroscopy, single photon counting technique, cyclic voltammetry, thermogravimetric analysis, and DFT calculations. Boruah et al. [48][49] developed an efficient method for the construction of regioisomeric 1,3,4-trisubstituted pyrazolo[3,4-b

Recent applications of click chemistry for the functionalization of gold nanoparticles and their conversion to glyco-gold nanoparticles

• Vivek Poonthiyil,
• Thisbe K. Lindhorst,
• Vladimir B. Golovko and
• Antony J. Fairbanks

Beilstein J. Org. Chem. 2018, 14, 11–24, doi:10.3762/bjoc.14.2

• , CHCl3, and THF. The broad peaks corresponding to the ligand ATT 33 protons in the 1H NMR spectra of the purified ATT-AuNPs (Supporting Information File 1, Figure S1) confirmed the attachment of the ATT 33 to the AuNPs. Thermogravimetric analysis of ATT-AuNPs (Figure S2) and the size distribution of Cit

Synthesis and application of trifluoroethoxy-substituted phthalocyanines and subphthalocyanines

• Satoru Mori and
• Norio Shibata

Beilstein J. Org. Chem. 2017, 13, 2273–2296, doi:10.3762/bjoc.13.224

• 10 to 72%) depending on the reaction conditions. A thermogravimetric analysis showed a weight loss of more than 90% at 210 °C for the precursor before condensation of TFEO-ZnPc, whereas the TFEO-ZnPc-supported fluoropolymer showed only 5% weight loss at 300 °C. It was suggested that introduction of

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

• thermogravimetric analysis (described below). 13C{1H} CP-MAS NMR. The solid-state NMR spectra of fisetin, γ-CD hydrate and γ-CD·fisetin are depicted in Figure 2. The spectrum of fisetin presents some well-resolved resonances that are ascribed to the carbonyl and C1, C7, C8, C9, and C6’ carbon atoms by comparison

• resonances that are observed in the region ascribed to the carbonyl of fisetin, indicating the occurrence of at least two different environments or inclusion geometries [35]. Thermogravimetric analysis (TG). In the TG studies, the samples were heated at a rate of 5 °C per min while registering changes in

• water-saturated chamber. The solid was allowed to rest inside this chamber overnight (ca. 16 hours). Anal. calcd for C48H80O40·C15H10O6·20H2O (1943.7): C, 38.93; H, 6.742; found: C, 38.77; H, 6.481. Thermogravimetric analysis up to 120 °C revealed a mass loss of 16%, corresponding to 17 water molecules

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

• content of ligands on the surface, thermogravimetric analysis was performed (TGA) after several centrifugation steps, as shown in Figure 4a. A total weight loss of 20% was determined. Although the particles were dried proper in high vacuum a shoulder around 200 °C shows up. This shoulder belongs to benzyl

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

• characterized by thermogravimetric analysis (TGA) under nitrogen atmosphere (Figure S4, Supporting Information File 1). The TGA plots show that the decomposition temperature of the polymers is at about 300 °C and there is 35% mass loss when the temperature reaches 800 °C, indicating good thermal stability of

Synthesis of three-dimensional porous hyper-crosslinked polymers via thiol–yne reaction

• Mathias Lang,
• Alexandra Schade and
• Stefan Bräse

Beilstein J. Org. Chem. 2016, 12, 2570–2576, doi:10.3762/bjoc.12.252

• crosslinking reaction conditions. The obtained HCPs showed BET surface areas up to 650 m²/g and are insoluble in common organic solvents. The characterisation of the networks was performed using IR spectroscopy, elemental analysis, thermogravimetric analysis (TGA), scanning electron microscopy (SEM), powder X

Hydroxy-functionalized hyper-cross-linked ultra-microporous organic polymers for selective CO₂ capture at room temperature

• Partha Samanta,
• Priyanshu Chandra and
• Sujit K. Ghosh

Beilstein J. Org. Chem. 2016, 12, 1981–1986, doi:10.3762/bjoc.12.185

• stretching frequencies of –OH groups and aromatic C=C double bonds, respectively (Figure 2a). Similar to the HCP-91, peaks corresponding to –OH groups and aromatic C=C double bonds were found at ≈3300–3500 cm−1 and ≈1643 and 1500 cm−1, respectively (Figure 2a). Meanwhile a thermogravimetric analysis (TGA

Star-shaped and linear π-conjugated oligomers consisting of a tetrathienoanthracene core and multiple diketopyrrolopyrrole arms for organic solar cells

• Hideaki Komiyama,
• Chihaya Adachi and
• Takuma Yasuda

Beilstein J. Org. Chem. 2016, 12, 1459–1466, doi:10.3762/bjoc.12.142

• cross-coupling reaction. Both TTA-DPP4 and TTA-DPP2 were soluble in common organic solvents, such as chloroform, toluene, and chlorobenzene. The thermal stability of these compounds was analyzed by thermogravimetric analysis (TGA). As shown in Figure 3, the 5% weight-loss temperature of TTA-DPP4 and TTA

• . Thermogravimetric analysis (TGA) was performed using a Hitachi High-Tech Science TG/DTA7300 with a heating rate of 10 °C min−1 under N2 atmosphere. UV–vis absorption spectra were recorded on a JASCO V-670Y spectrometer. Photoelectron yield spectra were recorded on a Riken-Keiki AC-2 ultraviolet photoelectron

Syntheses of dibenzo[d,d']benzo[2,1-b:3,4-b']difuran derivatives and their application to organic field-effect transistors

• Minh Anh Truong and
• Koji Nakano

Beilstein J. Org. Chem. 2016, 12, 805–812, doi:10.3762/bjoc.12.79

• stability of syn-DBBDF 5 and syn-DNBDF 6 were evaluated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), respectively. The DSC scans of syn-DBBDF 5 and syn-DNBDF 6 showed some transition peaks with the first phase-transition temperature at 20 °C and 45 °C, respectively, in

Interactions of cyclodextrins and their derivatives with toxic organophosphorus compounds

• Sophie Letort,
• Sébastien Balieu,
• William Erb,
• Géraldine Gouhier and
• François Estour

Beilstein J. Org. Chem. 2016, 12, 204–228, doi:10.3762/bjoc.12.23

• localized out of the larger rim of the TRIMEB cavity, the aromatic group slightly twisted out of the rim. In addition to the structural elucidation of this complex, isothermal and non-isothermal thermogravimetric analysis were performed. Obtained from the solid-state kinetic experiments, the relatively high

Synthesis and photophysical characteristics of polyfluorene polyrotaxanes

• Aurica Farcas,
• Giulia Tregnago,
• Ana-Maria Resmerita,
• Pierre-Henri Aubert and
• Franco Cacialli

Beilstein J. Org. Chem. 2015, 11, 2677–2688, doi:10.3762/bjoc.11.288

• polyrotaxanes than that of 3 non-rotaxane sample was assigned to the different content of threaded TM-βCD or TM-γCD on the copolymer chains (see incomplete coverage determined by 1H NMR). The thermal properties of the copolymers were evaluated by differential scanning calorimetry (DSC) and thermogravimetric

• analysis (TGA). All copolymers showed only glass-transitions (Tg) and not any exothermal crystallization peak characteristic of polymers containing 9,9-dioctyl-2,7-fluorene units (PFO) [49], Figure 2. The non-rotaxane copolymer 3 has a Tg at 88 °C. The Tg value increases for 3·TM-γCD and 3·TM-βCD to 96 °C

Consequences of the electronic tuning of latent ruthenium-based olefin metathesis catalysts on their reactivity

• Karolina Żukowska,
• Eva Pump,
• Aleksandra E. Pazio,
• Krzysztof Woźniak,
• Luigi Cavallo and
• Christian Slugovc

Beilstein J. Org. Chem. 2015, 11, 1458–1468, doi:10.3762/bjoc.11.158

• . Big symbols: thermogravimetric analysis (TGA); no symbols: differential scanning calorimetry (DSC). trans–cis Isomerization. Synthesis of the ligand precursors. Synthesis of the ruthenium complexes. Possible reaction pathways of 16. Supporting Information Supporting Information File 360: Full

Synthesis of tripodal catecholates and their immobilization on zinc oxide nanoparticles

• Franziska Klitsche,
• Julian Ramcke,
• Julia Migenda,
• Andreas Hensel,
• Tobias Vossmeyer,
• Horst Weller,
• Silvia Gross and
• Wolfgang Maison

Beilstein J. Org. Chem. 2015, 11, 678–686, doi:10.3762/bjoc.11.77

• catecholates and their immobilization on TiO2 and stainless steel. Experimental Synthesis The following compounds were synthesized according to literature procedures: 1 [42], 2 [31], 3 [31], 12 [42] 14 [46]. Thermogravimetric analysis The TGA data were obtained with a Pyris 1 TGA of Perkin Elmer under Nitrogen

Inclusion of trans-resveratrol in methylated cyclodextrins: synthesis and solid-state structures

• Lee Trollope,
• Dyanne L. Cruickshank,
• Terence Noonan,
• Susan A. Bourne,
• Milena Sorrenti,
• Laura Catenacci and
• Mino R. Caira

Beilstein J. Org. Chem. 2014, 10, 3136–3151, doi:10.3762/bjoc.10.331

• three crystalline inclusion complexes were also fully characterized by thermal analysis (hot stage microscopy, thermogravimetric analysis and differential scanning calorimetry). To complement the solid-state data, phase-solubility studies were conducted using a series of CDs (native and variously

• co-crystallization from different solutions, by co-evaporation using a rotavapor, or by exposure to microwave radiation. Characterization of the products was achieved using DSC and simultaneous thermogravimetric analysis (TGA/DSC), with support from FTIR spectroscopy and PXRD, where necessary. An

• prepare the binary systems. Differential scanning calorimetry (DSC) indicated that the commercial product melted at Tpeak,m = 266.3(4) °C (Tonset = 265.1(3) °C; ΔHm = 279(2) J g−1) (Figure 2, curve (a)). Thermogravimetric analysis (TGA) revealed mass loss only at 275 °C attributable to sample