Through-bond and through-space solid-state NMR correlation experiments at natural isotopic abundance (refocused cross-polarization incredible natural abundance double quantum transfer experiment (CPINADEQUATE), 1H-13C HETCOR, 1H-13C magic-angle spinning J heteronuclear multiple-quantum coherence (MAS-J-HMQC)) are presented on a moderately sized molecule of simavastatin (C25H38O5). Refocused 13C...

Various motionally averaged 31P-1H, 13C-1H, 1H-1H, and 31P-13C dipolar couplings were measured for natural-abundance and unoriented phosphocholine in the L alpha phase. The couplings were obtained and assigned by a variety of advanced and partly novel two-dimensional solid-state NMR experiments. Whereas 31P-1H and 31P-13C dipolar couplings provide long-range structural constraints, geminal 1H-1...

Using methanesulfonic acid as a catalyst, a series of cyclododeceno[b]indene derivatives were synthesized by the cyclization of alpha-benzylcyclododecanones, which were prepared by the reactions of cyclododecanones with a variety of substituted benzyl chlorides or bromides using NaH as a base. Their structures were confirmed by mp, IR spectra, 1H-NMR, 13C-NMR, MS, and x-ray diffraction. The pre...

Two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy has been used to assign 13C spectra of the tricyclic antidepressants imipramine and chlorimipramine . The 2DINADEQUATE method was used to unambiguously assign the aromatic spectral region for the former compound. Errors in previous literature assignments based on 1D methods were corrected. For chlorimipramine the pitfalls of class...

An efficient synthesis of vinylphosphonates is described. This involves the reaction of alkyl cyanoformates and dialkyl acetylendicarboxylates in the presence of trialkyl phosphites. The 1H, 13C NMR, and 31P NMR spectra of vinylphosphonates having different substitution are consistent with the presence of two geometrical isomers.

In isotropic solution, internuclear dipolar couplings average to zero as a result of rotational diffusion. By dissolving macromolecules in a dilute aqueous nematic discotic liquid-crystalline medium containing widely spaced magnetically oriented particles, a tunable degree of solute alignment with the magnetic field can be created while retaining the high resolution and sensitivity of the regul...

Despite obvious improvements in spectral resolution at high magnetic field, the detection of 13C labeling by 1H-[13C] NMR spectroscopy remains hampered by spectral overlap, such as in the spectral region of 1H resonances bound to C3 of glutamate (Glu) and glutamine (Gln), and C6 of N-acetylaspartate (NAA). The aim of this study was to develop, implement, and apply a novel 1H-[13C] NMR spectrosc...

The combination of different experimental techniques, such as solid 13C and 1H magic-angle spinning NMR spectroscopy, fluorescence spectroscopy and powder X-ray diffraction, together with theoretical calculations allows the determination of the unique structure directing the role of the bulky aromatic proton sponge 1,8-bis(dimethylamino)naphthalene (DMAN) towards the extra-large-pore ITQ-51 zeo...

In this paper, synthesis, single-crystal X-ray structure, Hirshfeld and DFT studies of 1,8-dichloro-9,10-dihydro-9,10-ethanoanthracene-11-carboxylic acid are discussed. Different intermolecular contacts affecting the crystal stability studied using calculations. The H…Cl O…H most significant, showing corresponding interaction distances 2.731 Å (Cl2…H10) 1.681Å (H1…O1), 2.328 (O1…H13), 2.510 (O1...

phytochemical investigation of the dichloromethane extract of the dried roots of ferula badrakema resulted in the identification of one new and six known compounds. known compounds were sesquiterpene coumarins: mogoltacin, feselol, badrakemin acetate, ferocaulidin, conferone and conferol acetate. the new compound was a sesquiterpene, named badrakemonin. the structures of these compounds were el...