A general and atom-efficient continuous-flow approach to prepare amines, amides and imines via reactive N-chloramines

• Katherine E. Jolley,
• Michael R. Chapman and
• A. John Blacker

Beilstein J. Org. Chem. 2018, 14, 2220–2228, doi:10.3762/bjoc.14.196

• -toluenesulfonamide (11) was investigated as substrate. Differential scanning calorimetry (DSC) was used to assess the thermal stability of 11, which melts at 78 °C and decomposes between 160–200 °C. This profile peaks at 188 °C, corresponding to an enthalpy of decomposition of −84.7 kJ mol−1 (see Supporting

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

• scanning calorimetry (DSC) under nitrogen atmosphere at a scanning rate of 10 °C/min and the results are shown in Figure 4. Both CEPDO and CBPDO show very high thermal stability with decomposition temperatures (Td) of 409 and 396 °C and glass transition temperatures (Tg) of 167 and 138 °C, respectively

• 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

Structure–property relationships and third-order nonlinearities in diketopyrrolopyrrole based D–π–A–π–D molecules

• Jan Podlesný,
• Lenka Dokládalová,
• Oldřich Pytela,
• Adam Urbanec,
• Milan Klikar,
• Numan Almonasy,
• Tomáš Mikysek,
• Jaroslav Jedryka,
• Iwan V. Kityk and
• Filip Bureš

Beilstein J. Org. Chem. 2017, 13, 2374–2384, doi:10.3762/bjoc.13.235

• of the peripheral substituents (donor) and enlargement of the π-system. Fundamental properties of target molecules were studied by differential scanning calorimetry, electrochemistry, and absorption and emission spectra. Nonlinear optical properties were studied by measuring the third harmonic

• were further investigated by differential scanning calorimetry (DSC), electrochemistry, absorption and emission spectra, DFT calculations, and THG measurements. Results and Discussion Synthesis of DPP derivatives 1–5 According to the π-linker structure, two series of target chromophores a and b can be

• chromatography without a need of further crystallization. Hence, this ferrocene derivative was prepared with the highest yield of 73%. In the solid state, all target chromophores resemble dark metallic solids. Differential scanning calorimetry The thermal behaviour of compounds 1–5b was studied by differential

Mechanochemical borylation of aryldiazonium salts; merging light and ball milling

• José G. Hernández

Beilstein J. Org. Chem. 2017, 13, 1463–1469, doi:10.3762/bjoc.13.144

• of the reaction mixture seemed homogeneous. Differential scanning calorimetry (DSC) analysis of the aryldiazonium salts 1a–d revealed that 1a–c melt followed by decomposition of the samples. However, the DSC profile of the iodobenzenediazonium salt 1d showed a direct thermal decomposition upon

Aggregation behaviour of a single-chain, phenylene-modified bolalipid and its miscibility with classical phospholipids

• Simon Drescher,
• Vasil M. Garamus,
• Christopher J. Garvey,
• Annette Meister and
• Alfred Blume

Beilstein J. Org. Chem. 2017, 13, 995–1007, doi:10.3762/bjoc.13.99

• was studied as a function of temperature using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), Fourier-transform infrared (FTIR) spectroscopy, and small angle neutron scattering (SANS). We show that our new bolalipid self-assembles into nanofibres, which transform into

• simulations [27]. A temperature increase leads to a transformation of the nanofibres into small micelles and the gel character is lost. This reversible gel/sol transformation is accompanied by a cooperative endothermic transition at Tm = 48 °C, which can be followed by differential scanning calorimetry (DSC

• Microscopy GmbH, Jena, Germany). Differential scanning calorimetry (DSC) DSC measurements were performed using a MicroCal VP-DSC differential scanning calorimeter (MicroCal Inc. Northampton, MA, USA). Before the measurements, the sample suspension and the water (or phosphate buffer) used as a reference were

A new class of organogelators based on triphenylmethyl derivatives of primary alcohols: hydrophobic interactions alone can mediate gelation

• Wangkhem P. Singh and
• Rajkumar S. Singh

Beilstein J. Org. Chem. 2017, 13, 138–149, doi:10.3762/bjoc.13.17

• acidic solution in contrast to its unstable solution-phase behavior. Differential scanning calorimetry Differential scanning calorimetry (DSC) of gels prepared from TPM-G12 (in propan-1-ol and DMSO) was carried out to study the gel-sol transition (Tgel) behaviour. Figure 3 shows the DSC heating curves of

Synthesis and evaluation of anti-oxidant and cytotoxic activities of novel 10-undecenoic acid methyl ester based lipoconjugates of phenolic acids

• Naganna Narra,
• Shiva Shanker Kaki,
• Rachapudi Badari Narayana Prasad,
• Sunil Misra,
• Koude Dhevendar,
• Venkateshwarlu Kontham and
• Padmaja V. Korlipara

Beilstein J. Org. Chem. 2017, 13, 26–32, doi:10.3762/bjoc.13.4

• by differential scanning calorimetry (DSC). DSC is a sensitive technique and has been used for investigating the thermotropic properties of several compounds including biological macromolecules, drugs and lipid-based materials for their stability and other characteristics [16]. In the present study

• is the absorbance of the tested sample after 40 min. DSC measurements The anti-oxidant activity was also evaluated by differential scanning calorimetry using pure linoleic acid as a lipid model system [23][24]. All studied anti-oxidants were dissolved in methanol to prepare 1 mM solutions. Samples of

• structures were confirmed by spectral data. The anti-oxidant activity of the synthesized lipoconjugates of phenolic acids was studied by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay and also by the inhibition of linoleic acid oxidation in micellar medium by differential scanning

Effects of solvent additive on “s-shaped” curves in solution-processed small molecule solar cells

• John A. Love,
• Shu-Hua Chou,
• Ye Huang,
• Guilllermo C. Bazan and
• Thuc-Quyen Nguyen

Beilstein J. Org. Chem. 2016, 12, 2543–2555, doi:10.3762/bjoc.12.249

• differential scanning calorimetry (DSC) and compared to its predecessor, p-SIDT(FBTTh2)2. A significant impact on thermal behaviors was observed upon substituting 2-hexylthiophene with octyl cyanoacetate (Supporting Information File 1, Figure S4 and Table S1). As compared to p-SIDT(FBTTh2)2, the melting (Tm

Comparing blends and blocks: Synthesis of partially fluorinated diblock polythiophene copolymers to investigate the thermal stability of optical and morphological properties

• Pierre Boufflet,
• Sebastian Wood,
• Jessica Wade,
• Zhuping Fei,
• Ji-Seon Kim and
• Martin Heeney

Beilstein J. Org. Chem. 2016, 12, 2150–2163, doi:10.3762/bjoc.12.205

• approach was not feasible. In that case, washing with dichloromethane resulted in a demonstrable removal of P3OT homopolymer, as indicated by the differential scanning calorimetry (DSC) thermogram (see Figure 1). Indeed, the melting peak around 190 °C, apparent in the crude block copolymer and attributable

• likely indicates less inter- and intrachain coupling, and possibly a frustration of the crystallization and phase separation in the case of these block copolymers. Thermal behavior Differential scanning calorimetry Fluorination of P3OT has previously been shown to result in a 50–60 °C increase in the

• , TCE-d2, 403 K, δ) 7.05 (s, 1H), 2.93–2.86 (m, 1.8H), 2.85–2.76 (m, 8.3H), 1.91–1.64 (m, 10.9H), 1.58–1.27 (m, 56.9H), 1.06–0.89 (m, 15.1H); 19F NMR (376 MHz, TCE-d2, 403 K, δ) −122.94 (s). Differential scanning calorimetry thermogram (second cycle, 10 K/min) of P3OT-b-F-P3OT 2:1 before (black) and

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

Amino-functionalized (meth)acryl polymers by use of a solvent-polarity sensitive protecting group (Br-t-BOC)

• Helmut Ritter,
• Monir Tabatabai and
• Markus Herrmann

Beilstein J. Org. Chem. 2016, 12, 245–252, doi:10.3762/bjoc.12.26

• spectrometer equipped with a diamond single bounce ATR accessory. The measurements were performed in the range of 400–3000 cm−1 at room temperature. Differential scanning calorimetry (DSC) was performed using a Mettler Toledo DSC 822 instrument equipped with a sample robot TSO801RO. The Apparatus was

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

• . Various analytical tests were used to access such information in the cases of pesticides [40][41][42]. Phase solubility diagrams could be obtained if changes of their water solubility upon inclusion occur, whereas differential scanning calorimetry (DSC) could be used to discriminate inclusion complexes

Thermal and oxidative stability of Atlantic salmon oil (Salmo salar L.) and complexation with β-cyclodextrin

• Daniel I. Hădărugă,
• Mustafa Ünlüsayin,
• Alexandra T. Gruia,
• Cristina Birău (Mitroi),
• Gerlinde Rusu and
• Nicoleta G. Hădărugă

Beilstein J. Org. Chem. 2016, 12, 179–191, doi:10.3762/bjoc.12.20

• -CD/ASO complexes. The analysis of the complexes by thermogravimetry, differential scanning calorimetry (DSC), and Karl Fischer titration (KFT) as well as the decrease of the “strongly-retained” water content confirm the formation of the inclusion compound. Furthermore, the DSC parameters correlate

• well with the KFT kinetic data for β-CD/ASO complexes. Keywords: Atlantic salmon oil (ASO); β-cyclodextrin; differential scanning calorimetry; Karl Fischer titration; omega-3 fatty acid; thermogravimetry; Introduction Functional food products containing omega-3 supplementation are becoming more and

• water and solvent contents in host–guest supramolecular systems by thermal analyses have already been performed for CD/flavonoid and CD/essential oil complexes [37][39]. Differential scanning calorimetry (DSC) analysis DSC can provide further information on the physical and chemical processes occurring

Physical properties and biological activities of hesperetin and naringenin in complex with methylated β-cyclodextrin

• Waratchada Sangpheak,
• Jintawee Kicuntod,
• Roswitha Schuster,
• Thanyada Rungrotmongkol,
• Peter Wolschann,
• Nawee Kungwan,
• Helmut Viernstein,
• Monika Mueller and
• Piamsook Pongsawasdi

Beilstein J. Org. Chem. 2015, 11, 2763–2773, doi:10.3762/bjoc.11.297

• diagram showed the formation of a soluble complex of AL type, with higher increase in solubility and stability when hesperetin and naringenin were complexed with RAMEB. Solid complexes were prepared by freeze-drying, and the data from differential scanning calorimetry (DSC) confirmed the formation of

• 24 hours. The dried powder was stored in desiccators for further use. Differential scanning calorimetry (DSC) analysis The differential scanning calorimetry (DSC, Netzsch, 204 F1 Phoenix) was used for recording DSC thermograms of the free hesperetin and naringenin and the inclusion complexes with β

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

Inclusion complexes of 2-methoxyestradiol with dimethylated and permethylated β-cyclodextrins: models for cyclodextrin–steroid interaction

• Mino R. Caira,
• Susan A. Bourne,
• Halima Samsodien and
• Vincent J. Smith

Beilstein J. Org. Chem. 2015, 11, 2616–2630, doi:10.3762/bjoc.11.281

• well-defined and hence met the criterion for subsequent solubility studies. Interaction between 2ME and the amorphous CD derivatives RAMEB and HPBCD PXRD, differential scanning calorimetry (DSC) and FTIR methods were employed to investigate the products of kneading between crystalline 2ME and these

Cross-metathesis of polynorbornene with polyoctenamer: a kinetic study

• Yulia I. Denisova,
• Maria L. Gringolts,
• Alexander S. Peregudov,
• Liya B. Krentsel,
• Ekaterina A. Litmanovich,
• Arkadiy D. Litmanovich,
• Eugene Sh. Finkelshtein and
• Yaroslav V. Kudryavtsev

Beilstein J. Org. Chem. 2015, 11, 1796–1808, doi:10.3762/bjoc.11.195

• MHz (13C NMR); CDCl3 (Aldrich) was used as solvent. Chemical shifts δ were reported in parts per million relative to the residual CHCl3 signal as an internal reference standard. Differential scanning calorimetry (DSC) thermograms were recorded on a Mettler TA 4000 system at a rate of 10 °C/min under

Thermal properties of ruthenium alkylidene-polymerized dicyclopentadiene

• Yuval Vidavsky,
• Yotam Navon,
• Yakov Ginzburg,
• Moshe Gottlieb and
• N. Gabriel Lemcoff

Beilstein J. Org. Chem. 2015, 11, 1469–1474, doi:10.3762/bjoc.11.159

• Differential scanning calorimetry (DSC) analysis of ring opening methatesis polymerization (ROMP) derived polydicyclopentadiene (PDCPD) revealed an unexpected thermal behavior. A recurring exothermic signal can be observed in the DSC analysis after an elapsed time period. This exothermic signal was found to be

• of 98.9% at polymerization temperatures of 60 °C with the Grubbs first generation catalyst. By carrying out detailed differential scanning calorimetry (DSC) analyses Kessler and Mauldin [27] demonstrated a sharp exothermic peak related to the heat of reaction and a final Tg of 164 °C at conversions

• observations. Experimental All commercially available chemicals were of reagent grade quality and used without further purification, unless described. Differential scanning calorimetry (DSC) data was obtained using a METTLER-TOLEDO DSC 823 and results were evaluated with the STARe software. All experiments

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

Selected synthetic strategies to cyclophanes

• Sambasivarao Kotha,
• Mukesh E. Shirbhate and
• Gopalkrushna T. Waghule

Beilstein J. Org. Chem. 2015, 11, 1274–1331, doi:10.3762/bjoc.11.142

• synthesized hexa-peri-hexabenzocoronene cyclophane 201a–c. They studied their properties by carrying out differential scanning calorimetry (DSC), optical microscopy, wide-angle X-ray scattering (WAXD), and scanning tunneling microscopy (STM). Tunneling spectroscopy reveals a diode-like behavior which

Synthesis of photoresponsive cholesterol-based azobenzene organogels: dependence on different spacer lengths

• Yuchun Ren,
• Bin Wang and
• Xiuqing Zhang

Beilstein J. Org. Chem. 2015, 11, 1089–1095, doi:10.3762/bjoc.11.122

• spectra were recorded using a spectrophotometer (UV-3600, Shimadzu, Japan). Differential scanning calorimetry (DSC) was carried out on a thermal analysis (TA) DSC-Q30 in nitrogen at a heating rate of 10 K/min. Synthetic procedures Synthesis of m2–m12. 3β-[(2-hydroxyethyl)oxy]cholest-5-ene (m2) was

• shown in Supporting Information File 1, Figures S1–S4. M3 and M10 have the photochromic properties. Liquid crystal properties of the synthesized compounds The structures of these compounds are shown in Scheme 1. The thermal behaviors of the seven compounds were analyzed by differential scanning

• calorimetry (DSC). The DSC curves of the cholesterol-based supramolecular complexes are shown in Figure 2 and phase transition temperatures are listed in Table 1. The DSC thermogram of M0 presented three peaks at 158, 211 and 249 °C on heating, corresponding to the crystal to crystal transition, crystal to

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

• 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

• a mortar with a pestle, and passed through a 250 μm sieve. Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) For the binary systems investigated, temperature and enthalpy values were measured with a Mettler STARe system (Mettler Toledo, Novate Milanese, MI, Italy) equipped

Modification of physical properties of poly(L-lactic acid) by addition of methyl-β-cyclodextrin

• Toshiyuki Suzuki,
• Ayaka Ei,
• Yoshihisa Takada,
• Hiroki Uehara,
• Takeshi Yamanobe and
• Keiko Takahashi

Beilstein J. Org. Chem. 2014, 10, 2997–3006, doi:10.3762/bjoc.10.318

• containing approximately 17% MeCD was drawn to more than 1000% at 60 °C, although PLLA fractured at a strain of less than 100%. Differential scanning calorimetry (DSC)-Raman in situ measurements also revealed decreases in the glass transition temperature (Tg), cold crystallization temperature (Tc), and

• necessary to acquire information about their thermal properties and structure. Differential scanning calorimetry (DSC) is a very useful method for analyzing the thermal properties such as Tg and cold crystallization temperature (Tc). However, it does not provide details about the structural change. On the

Synthesis and properties of novel star-shaped oligofluorene conjugated systems with BODIPY cores

• Clara Orofino-Pena,
• Diego Cortizo-Lacalle,
• Joseph Cameron,
• Muhammad T. Sajjad,
• Pavlos P. Manousiadis,
• Neil J. Findlay,
• Alexander L. Kanibolotsky,
• Dimali Amarasinghe,
• Peter J. Skabara,
• Tell Tuttle,
• Graham A. Turnbull and
• Ifor D. W. Samuel

Beilstein J. Org. Chem. 2014, 10, 2704–2714, doi:10.3762/bjoc.10.285

• Information File 1). The morphological stability was evaluated by differential scanning calorimetry (DSC). All of the synthesised compounds were found to be amorphous materials and exhibited reasonably high glass transition temperatures (Tg) (Table 1, Figure S2, Supporting Information File 1). The Tg value

• Perkin-Elmer Thermogravimetric Analyser TGA7 under a constant flow of argon. Differential Scanning Calorimetry (DSC) was conducted on a TA Instruments Q1000 with a RC-90 refrigerated cooling unit attached. The calibration was conducted using indium (melt temperature 156.42 °C, ∆Hf 28.42 J/g). The test