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Plenthora of glycosylation reactions was performed and sophisticated NMR approach for characteriza-tion of the coressponding products was aplied. ID 19F and *H NMR were utilized for accurate derermina-tion of anomeric ratios and 2D NMR techniques as HSQC, HMBC and COSY were used to assign the signals of individual anomers. In some cases, spectrum simulation was necessary to obtain the desired parameters.

Determining how organic molecules self-assemble into a solid material is a challenging and demanding task if a single crystal of the material cannot be produced. Solid-state NMR spectroscopy offers access to such molecular details via an appropriate selection of techniques. This report gives a selected overview of 1D and 2D solid-state NMR techniques for elucidating the structure of soft organic solids. We focus on how the solid-state NMR techniques are designed from the perspective of the different nuclear interactions, using average Hamiltonian theory and product operators. We also introduce recent methods for quantification and reduction of experimental artifacts. Finally, we highlight how the solid-state NMR techniques can be applied to soft organic materials by reviewing recent applications to semicrystalline polymers, pi-conjugated polymers, natural silk, and graphene-related materials.

In the synthesis of N-alkylaminoalkanethiosulfuric acids, there exists the possibility of forming two products in the last step of the synthesis. In the case of the seven acids synthesized in this laboratory from styrene oxide and primary aliphatic amines, the common spectroscopic methods were inadequate for distinguishing which of the two isomers was obtained. Carbon-13 chemical shift calculations employing the ACD/CNMR program were helpful, but not conclusive for identifying the products. The use of HMQC, HMBC and TOCSY techniques permitted the identification of the products as the 2-(N-alkylamino)-1-phenyl-1-ethanethiosulfuric acids. Na obtenção de ácidos N-alquilaminoalcanotiossulfúricos, existe a possibilidade de formação de dois produtos na última etapa da síntese. No caso dos sete ácidos sintetizados neste laboratório a partir de óxido de estireno e aminas primárias alifáticas, os métodos comuns de espectroscopia não foram adequados para distinguir qual dos dois isômeros foi formado. Cálculos de deslocamentos químicos de carbono-13 empregando o programa ACD/CNMR ajudaram, mas não foram conclusivos para a identificação dos produtos. O uso de técnicas como HMQC, HMBC e TOCSY permitiu a identificação dos produtos como os ácidos 2-(N-alquilamino)-1-phenyl-1-etanotiossulfúricos.

Saponins are oligoglycosides with spirostane, steroid or triterpenoid aglycones as their genins, which constitute an important kind of natural product. Some of them exhibit prominent bioactivities, such as the saponins from Panax ginseng and Glycyrrhiza uralensis. Because of their high polarity and relatively complicated structures, it was time- and sample-consuming work to purify and identify them before the 1980’s. In the past decade, the continuing development of various advanced chromatographic materials and spectroscopic methods have made it possible to isolate and determine the structures of certain minor saponins ocurring only in small quantities in a short time.