Nuclear magnetic resonance spectral analysis of polymer-supported reagents and catalysts

Abstract

High resolution and cross-polarisation/magic angle spinning nuclear magnetic resonance spectroscopy of crosslinked polystyrene and of reagents and catalysts supported on crosslinked polystyrene and silica gel are reviewed. The materials studied include ionexchange resins, resins in solid phase pep tide synthesis, organic synthetic reagents, phase transfer catalysts, transition metal catalysts, and liquid chromatography column packings. 13C and 3 1 P n.m.r. spectra have been used to identify structures and to study macromolecule and micromolecule dynamics. New spectra of crosslinked polystyrenes and supported reagents are reported. Procedure to obtain qualitative and quantitative spectra are recommended.

Solid-Phase Organic Synthesis: A Critical Understanding of the Resin

“…A review detailing early work on the application of NMR to crosslinked polymers has appeared. 79 Narrow signals in NMR (and EPR) spectra are only achieved if magnetic interactions between neighboring nuclei are averaged by random motion that is faster than the internuclear dipolar relaxation pathways. 80 This is readily attained in solution, but when affixed to large, static molecules, rapid motion of the dipoles becomes difficult.…”

Synthesis of Polymer Supported Lignin Model Compounds. Part 2. Use of the Wittig reaction in Attaching of Aldehyde Group Containing Lignin Model Compounds to Polystyrene

“…All I3 CNMR spectra were recorded fully decoupled using WALZ-1 6 and referenced to tetramethylsilane. The polymer spectra were recorded with the method of Ford et al (1984). Mass spectra were recorded on a Jeol JMS-SGX102 mass spectrometer.…”

“…L). We used 2% cross linked polystyrene because we wanted to monitor the chemical structure of polymer supported lignin model compounds by I3 C NMR (Ford et al 1984).…”

Synthesis and structure of metal complexes with organic polymers or inorganic supports

“…The preparation of the two functionalized resins was carried out by using classical reactions for the modification of polystyrene polymers (Ref. 15). In this way microporous and macroporous resins containing 0.01 to 0.2 mmol of chelating groups per gram were obtained from starting materials having crosslinking degree 4.5-6.3, surface area 38-750 m2/g ad average pore diameter 40-300 A.…”