Extrusion – back to the future: Using an established technique to reform automated chemical synthesis

• Deborah E. Crawford

Beilstein J. Org. Chem. 2017, 13, 65–75, doi:10.3762/bjoc.13.9

• literature demonstrating the utilisation of near-infrared spectroscopy for online monitoring to determine where in the extruder the cocrystal begins to form. Consequently this also provides feedback regarding screw configuration and deductions can be made as to whether sufficient mechanical energy is being

Towards potential nanoparticle contrast agents: Synthesis of new functionalized PEG bisphosphonates

• Souad Kachbi-Khelfallah,
• Maelle Monteil,
• Margery Cortes-Clerget,
• Evelyne Migianu-Griffoni,
• Jean-Luc Pirat,
• Olivier Gager,
• Julia Deschamp and
• Marc Lecouvey

Beilstein J. Org. Chem. 2016, 12, 1366–1371, doi:10.3762/bjoc.12.130

• at room temperature after 24 hours (Table 1, entries 8–10). The completion of the reaction was monitored by infrared spectroscopy with the disappearance of the hydroxy absorption band and the shifting of the carbonyl vibration band to about 1800 cm−1. The addition of two equivalents of tris

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

• sensitive components, e.g., drugs, proteins, DNA may be present without being affected. Experimental Methods 1H NMR measurements were performed using a Bruker Avance 300 operating at 300 MHz at room temperature. Fourier transformation infrared spectroscopy (FTIR) was performed on a Nicolet 6700 FTIR

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

• investigated to gain insight into CD–steroid interaction modes and the stability of the resulting inclusion complexes. These researchers also used Fourier transform infrared spectroscopy (FTIR), thermal analysis and powder X-ray diffraction (PXRD) to infer the existence of solid native CD–steroid inclusion

A new and efficient procedure for the synthesis of hexahydropyrimidine-fused 1,4-naphthoquinones

• Marcelo Isidoro P. Reis,
• Vinícius R. Campos,
• Jackson A. L. C. Resende,
• Fernando C. Silva and
• Vitor F. Ferreira

Beilstein J. Org. Chem. 2015, 11, 1235–1240, doi:10.3762/bjoc.11.137

• N,S-acetals. These compounds were obtained in good yields, and several of them showed promising antibacterial activity [42]. The structures of the synthesized 1,3,5-triazinanes were confirmed by spectroscopic techniques such as NMR, 1H and 13C-APT, infrared spectroscopy (FTIR) and high resolution

• temperature of 150 °C, the desired products were obtained in good yields (75–80%, Scheme 2). All structures of the benzo-fused tetrahydroquinazolines were characterized by 1H NMR and 13C-APT, infrared spectroscopy (FTIR) and high resolution mass spectrometry. Using compound 23 as an example, it can be

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

• described elsewhere [28]. General measurements NMR spectra were recorded with a Bruker-400 NMR spectrometer. Powder X-ray diffraction (XRD) measurements were carried out on a Rigaku D/max 2500PC (Japan)-type single-crystal diffractometer using Cu Kα radiation to determine the crystal structure. Infrared

• spectroscopy (IR) was measured on a Nicolet 6700 spectrometer from 4000 to 500 cm−1 at room temperature. The samples were prepared as KBr pellets. The morphology of the gel samples were examined by scanning electron microscopy (SEM, S5200, FEI Company) under an acceleration voltage of 30 kV. UV–vis absorption

Carboxylated dithiafulvenes and tetrathiafulvalene vinylogues: synthesis, electronic properties, and complexation with zinc ions

• Yunfei Wang and
• Yuming Zhao

Beilstein J. Org. Chem. 2015, 11, 957–965, doi:10.3762/bjoc.11.107

• properties of the coordination polymer were investigated by infrared spectroscopy, cyclic voltammetry, powder X-ray diffraction, and differential scanning calorimetric analyses. Furthermore, the microscopic porosity and surface area of the Zn-TTFV coordination polymer were measured by nitrogen gas adsorption

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

• gas flow. The samples were heated at 80 °C isothermally for 10 minutes and subsequently heated from 80 °C to 700 °C at a rate of 10 °C per minute. The experiments were carried out at least two times. Fourier transformation infrared spectroscopy IR spectra were measured on a Jasco FTIR 4100 device as a

IR and electrochemical synthesis and characterization of thin films of PEDOT grown on platinum single crystal electrodes in [EMMIM]Tf₂N ionic liquid

• Andrea P. Sandoval,
• Marco F. Suárez-Herrera and
• Juan M. Feliu

Beilstein J. Org. Chem. 2015, 11, 348–357, doi:10.3762/bjoc.11.40

• , E-03080 Alicante, Spain 10.3762/bjoc.11.40 Abstract Thin films of PEDOT synthesized on platinum single electrodes in contact with the ionic liquid 1-ethyl-2,3-dimethylimidazolium triflimide ([EMMIM]Tf2N) were studied by cyclic voltammetry, chronoamperometry, infrared spectroscopy and atomic force

• analyzed by in situ infrared spectroscopy, the observed bands depend on the applied potential. The reference potential in this case was −0.9 V in order to start form the neutral form of PEDOT. Therefore, the positive bands correspond to products present in the oxidized form while the negative bands

• Instruments) were used. In situ Fourier Transform Infrared spectroscopy (FTIR) experiments were performed with a Nexus 8700 (Thermo Scientific) spectrometer equipped with an MCT detector. The spectroelectrochemical cell was provided with a prismatic CaF2 window beveled at 60°. Spectra shown are composed of

Detonation nanodiamonds biofunctionalization and immobilization to titanium alloy surfaces as first steps towards medical application

• Juliana P. L. Gonçalves,
• Afnan Q. Shaikh,
• Manuela Reitzig,
• Daria A. Kovalenko,
• Jan Michael,
• René Beutner,
• Gianaurelio Cuniberti,
• Dieter Scharnweber and
• Jörg Opitz

Beilstein J. Org. Chem. 2014, 10, 2765–2773, doi:10.3762/bjoc.10.293

• material properties towards biomedical applications the authors aim to increase adhesion to bone material by incorporating nanodiamonds into the implant surface, namely the anodically grown titanium dioxide layer. Differently functionalized nanodiamonds are characterized by infrared spectroscopy and the

• character of binding of amino and phosphate groups. The obtained products were characterized by infrared spectroscopy. Figure 2 depicts the IR spectra of samples with phosphate groups coupled to the surface of the nanodiamond which use O-phosphorylethanolamine as main reagent. Figure 3 shows the infrared

• , with the main aim to couple phosphate groups. Successful DND functionalization was confirmed by infrared spectroscopy, depicting the presence of the attached functional groups at the DND surface. SEM results show better adhesion and homogeneous immobilization on the titanium alloy for the nanodiamonds

Linear-g-hyperbranched and cyclodextrin-based amphiphilic block copolymer as a multifunctional nanocarrier

• Yamei Zhao,
• Wei Tian,
• Guang Yang and
• Xiaodong Fan

Beilstein J. Org. Chem. 2014, 10, 2696–2703, doi:10.3762/bjoc.10.284

• ), further indicating that the pseudo-one-step method was effective in this reaction. Although the structure of P2 is relatively complicated, 1H nuclear magnetic resonance (NMR), 13C NMR, and Fourier transform infrared spectroscopy (FTIR) spectra can still be used to confirm the existence of characteristic

Loose-fit polypseudorotaxanes constructed from γ-CDs and PHEMA-PPG-PEG-PPG-PHEMA

• Tao Kong,
• Lin Ye,
• Ai-ying Zhang and
• Zeng-guo Feng

Beilstein J. Org. Chem. 2014, 10, 2461–2469, doi:10.3762/bjoc.10.257

• permeation chromatographic (GPC) measurements were carried out at 40 °C on a HLC-8320GPC (TOSOH, Japan) instrument using THF as eluent at a flow rate of 0.3 mL/min. All of the GPC data were calibrated using polystyrene (PS) standards. Fourier transform infrared spectroscopy (FTIR) spectra were measured using

Conformational analysis of 2,2-difluoroethylamine hydrochloride: double gauche effect

• Josué M. Silla,
• Claudimar J. Duarte,
• Rodrigo A. Cormanich,
• Roberto Rittner and
• Matheus P. Freitas

Beilstein J. Org. Chem. 2014, 10, 877–882, doi:10.3762/bjoc.10.84

• through theoretical calculations and infrared spectroscopy [11]. No significant double gauche effect has been found in 1, since conformers possessing two fluorine atoms in the gauche relationship with the amino group (gauche-gauche, gg) are estimated to be similarly populated to those conformers with only

Self-assembled organic–inorganic magnetic hybrid adsorbent ferrite based on cyclodextrin nanoparticles

• Ângelo M. L. Denadai,
• Frederico B. De Sousa,
• Joel J. Passos,
• Fernando C. Guatimosim,
• Kirla D. Barbosa,
• Ana E. Burgos,
• Fernando Castro de Oliveira,
• Jeann C. da Silva,
• Bernardo R. A. Neves,
• Nelcy D. S. Mohallem and
• Rubén D. Sinisterra

Beilstein J. Org. Chem. 2012, 8, 1867–1876, doi:10.3762/bjoc.8.215

• /Zn and the MHM prepared by using Fe-Ni/Zn and βCD (Fe-Ni/Zn/βCD) were synthesized by adapting a method previously described in the literature [7]. These magnetic materials were characterized in the solid state by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and

Cyanoethylation of the glucans dextran and pullulan: Substitution pattern and formation of nanostructures and entrapment of magnetic nanoparticles

• Kathrin Fiege,
• Heinrich Lünsdorf,
• Sevil Atarijabarzadeh and
• Petra Mischnick

Beilstein J. Org. Chem. 2012, 8, 551–566, doi:10.3762/bjoc.8.63

• infrared spectroscopy (ATR–IR). Gas–liquid chromatography (GLC) in combination with mass spectrometry (MS) was employed for the analysis of glucose derivatives after depolymerization of the cyanoethylglucans. The DS of heterogenic atoms containing polysaccharide derivatives can be followed by elementary

Air-stable, recyclable, and time-efficient diphenylphosphinite cellulose-supported palladium nanoparticles as a catalyst for Suzuki–Miyaura reactions

• Qingwei Du and
• Yiqun Li

Beilstein J. Org. Chem. 2011, 7, 378–385, doi:10.3762/bjoc.7.48

• in ethanol (Scheme 1). The as-prepared Cell–OPPh2–Pd0 catalyst was characterized by inductively coupled plasma-atomic emission spectrometry (ICP-AES), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analyses (TGA), scanning electron microscopy (SEM) and

Miniemulsion polymerization as a versatile tool for the synthesis of functionalized polymers

• Daniel Crespy and
• Katharina Landfester

Beilstein J. Org. Chem. 2010, 6, 1132–1148, doi:10.3762/bjoc.6.130

• nanoparticles prepared in inverse microemulsion [123]. The polyamide was identified by infrared spectroscopy. Polyimide nanoparticles could be synthesized in ionic liquids at temperatures up to 190 °C even although water is produced during the polycondensation as shown in Scheme 2 [15]. Here again, the reaction

Intramolecular hydroxycarbene C–H-insertion: The curious case of (o-methoxyphenyl)hydroxycarbene

• Dennis Gerbig,
• David Ley,
• Hans Peter Reisenauer and
• Peter R. Schreiner

Beilstein J. Org. Chem. 2010, 6, 1061–1069, doi:10.3762/bjoc.6.121

• trapped in an excess of Ar at 11 K and characterized by infrared spectroscopy. The insertion process kinetically outruns the alternative [1,2]H-tunneling reaction to o-anisaldehyde, a type of reaction observed for other hydroxycarbenes. Traces of the dehydration product, benzo[b]furan, were also detected

Expanding the gelation properties of valine-based 3,5-diaminobenzoate organogelators with N-alkylurea functionalities

• Hak-Fun Chow and
• Chin-Ho Cheng

Beilstein J. Org. Chem. 2010, 6, 1015–1021, doi:10.3762/bjoc.6.114

• also prevented the organogelators from crystallizing by imposing a higher degree of local disorder. Fourier transform infrared spectroscopy (FT-IR) was employed to elucidate the extent of intermolecular hydrogen bonding in the different macroscopic phases of organogelator 2 (n = 20) in o-xylene (Table