Mechanochemical bottom-up synthesis of phosphorus-linked, heptazine-based carbon nitrides using sodium phosphide

• Blaine G. Fiss,
• Georgia Douglas,
• Michael Ferguson,
• Jorge Becerra,
• Jesus Valdez,
• Trong-On Do,
• Tomislav Friščić and
• Audrey Moores

Beilstein J. Org. Chem. 2022, 18, 1203–1209, doi:10.3762/bjoc.18.125

• , mechanochemical synthesis of phosphorus-bridged heptazine-based carbon nitrides (g-h-PCN). The structure of these materials was determined through a combination of powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), 31P magic angle spinning nuclear magnetic resonance (MAS NMR), density

• at 300 °C for 1 hour under argon, the phosphorus content is shown to increase, while still remaining partially localized, with the particles retaining their size and morphology (Supporting Information File 1, Figure S4b). 31P magic angle spinning (MAS) NMR Bulk solid-state analysis of the heptazine

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

• via a 13C magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR) 1H-13C-CP experiment. An overall information of the compound is obtained by attenuated total reflection infrared spectroscopy (ATR-IR). Figure 1 shows the results of the characterization exemplarily for the fullerenol

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

• ) mode. FTIR spectra were recorded on a Thermo Scientific Nicolet iS10 spectrometer equipped with a Smart iTR diamond ATR sampling accessory in the range of 4000–650 cm−1. Solid-state NMR, 13C cross-polarization (CP)/magic angle spinning (MAS, 99.5 MHz) measurements were performed on a JEOL JNM-ECX 400

Dynamics and interactions of ibuprofen in cyclodextrin nanosponges by solid-state NMR spectroscopy

• Monica Ferro,
• Franca Castiglione,
• Nadia Pastori,
• Carlo Punta,
• Lucio Melone,
• Walter Panzeri,
• Barbara Rossi,
• Francesco Trotta and
• Andrea Mele

Beilstein J. Org. Chem. 2017, 13, 182–194, doi:10.3762/bjoc.13.21

• nanoporous polymer structure influences the delivery property of entrapped drugs [8]. In particular the transport properties of ibuprofen sodium salt (IbuNa) entrapped in CDNS polymer gels has been investigated by high resolution magic angle spinning (HR-MAS) NMR technique [9] as a paradigmatic case of an

• and line-width, may fail to provide an acceptable characterization due to high structural similarity at molecular level. Finally yet importantly, in the present work we also report on solid state 1H NMR spectra of the examined compounds acquired under fast magic angle spinning (Fast MAS) conditions

Cross-linked cyclodextrin-based material for treatment of metals and organic substances present in industrial discharge waters

• Élise Euvrard,
• Nadia Morin-Crini,
• Coline Druart,
• Justine Bugnet,
• Bernard Martel,
• Cesare Cosentino,
• Virginie Moutarlier and
• Grégorio Crini

Beilstein J. Org. Chem. 2016, 12, 1826–1838, doi:10.3762/bjoc.12.172

• magic angle spinning (CPMAS) spectrum shows the peaks of disordered cyclodextrin (broad signals) in the range of 50–110 ppm. Three strong broad bands attributable to the glucopyranose unit can be observed. The peak at 101 ppm is attributed to the anomeric carbon C-1: this confirms the presence of

• such as cross polarization magic angle spinning (CP MAS) and MAS. The spectra were recorded with a Bruker spectrometer operating at 75.47 MHz and 303 K. The compounds were placed in a zirconium rotor, 4 mm in diameter and 21 mm high. The chemical shifts were recorded relative to tetramethylsilane with

Polydisperse methyl β-cyclodextrin–epichlorohydrin polymers: variable contact time ¹³C CP-MAS solid-state NMR characterization

• Isabelle Mallard,
• Davy Baudelet,
• Franca Castiglione,
• Monica Ferro,
• Walter Panzeri,
• Enzio Ragg and
• Andrea Mele

Beilstein J. Org. Chem. 2015, 11, 2785–2794, doi:10.3762/bjoc.11.299

• obtained and characterized by solid-state 13C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS) conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials

• different amounts of imprinting agent, as in the present case. We herein propose an approach based on solid-state 13C NMR techniques such as variable contact time cross-polarization magic angle spinning with dipolar decoupling (VCP-MAS) to describe these new materials. The dynamics of cross-polarization can

Anomalous diffusion of Ibuprofen in cyclodextrin nanosponge hydrogels: an HRMAS NMR study

• Monica Ferro,
• Franca Castiglione,
• Carlo Punta,
• Lucio Melone,
• Walter Panzeri,
• Barbara Rossi,
• Francesco Trotta and
• Andrea Mele

Beilstein J. Org. Chem. 2014, 10, 2715–2723, doi:10.3762/bjoc.10.286

• ratio. The entrapment of IP was achieved by swelling the two polymers with a 0.27 M solution of IP in D2O, leading to colourless, homogeneous hydrogels loaded with IP. The molecular environment and the transport properties of IP in the hydrogels were studied by high resolution magic angle spinning

• confined drug inside the polymeric network, especially in the gel state. To this end, the use of high resolution magic angle spinning (HRMAS) NMR spectroscopy [20] opened the possibility of using the whole repertoire of NMR experiments to spot on the structural and dynamic properties of the drug entrapped

• used to investigate transport phenomena in heterogeneous systems endowed with liquid-like dynamics by applying pulsed field gradient spin echo (PGSE) methodologies under magic-angle spinning conditions [23]. This point is of great interest in the field of controlled release of active pharmaceutical

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

• and tetramethylsilane (TMS) as an internal standard. 13C cross-polarization magic-angle spinning (CP/MAS) NMR spectra were measured on a Bruker AV 300 NMR spectrometer with a single contact time of 1 ms and a spinning rate of 5 kHz. Chemical shifts were compared to an external adamantane standard. Gel

The chemistry of bisallenes

• Henning Hopf and
• Georgios Markopoulos

Beilstein J. Org. Chem. 2012, 8, 1936–1998, doi:10.3762/bjoc.8.225

A practical synthesis of the ¹³C/¹⁵N- labelled tripeptide N-formyl- Met-Leu-Phe, useful as a reference in solid- state NMR spectroscopy

• Sven T. Breitung,
• Jakob J. Lopez,
• Gerd Dürner,
• Clemens Glaubitz,
• Michael W. Göbel and
• Marcel Suhartono

Beilstein J. Org. Chem. 2008, 4, No. 35, doi:10.3762/bjoc.4.35

• 13C/15N-labelled tripeptide 1 could be isolated in a typical batch. This peptide can be easily crystallised and is therefore well suited as a standard sample for setting up solid-state NMR experiments. Keywords: Fmoc solid phase peptide synthesis; formylation; f-MLF; magic-angle spinning; Wang resin