By Walther L.

Oxidations, mark downs, and miscellaneous transformations of natural compounds with electrical energy in resolution and through silent electrical discharge.

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While specific applications of gel-phase NMR have been useful for SPS reaction monitoring, the great potential of SPS NMR is in the determination of structure and the measurement of purity and yields, especially through the use of magic angle spinning–high-resolution (MAS–HR) NMR techniques. 6. 5 On-Bead Methods: Mass Spectrometry The use of mass spectrometry (MS) techniques to monitor SP reactions has recently become possible through the use of matrix-assisted laser desorption/ionization–time of flight (MALDI–TOF) spectrometry (137) after in situ cleavage of a small number of resin beads (138–140).

20); the so-called analytical construct also allowed the photolytic release for analytical determinations of a larger fragment containing the target molecule, the acid linker, and a free amine (site 2, Fig. 20). The amine acted as a mass sensitizer, increased the MS signal of the reaction product, and via an isotopic labeling protocol (146) allowed to discard the MS signals of unbound materials; a single bead was largely enough to determine the quality of the reaction and to spot elusive side products (147, 148).

2 Selection of commerically available functional groups grafted onto PS resins. 2 a Note: THF = tetrahydrofuran; DMF = dimethyl formamide; DCM = dichloromethane. b Resin swelling measured as volume increase in respect to the dry bead. chemistry, which may be due to the leakage of PEG chains due to the use of aggressive reagents such as strong electrophiles or to the use of Lewis acids, which can form complexes with the PEG chains. The general tendency is to use PEG–PS resins for detailed SP studies, where reaction monitoring by NMR is necessary or when polar protic solvents are required.

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