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Application of HRMAS 1H NMR Spectroscopy To Investigate Interactions between Ligands and Synthetic Receptors

✍ Scribed by Heidi Händel; Elke Gesele; Klaus Gottschall; Klaus Albert


Publisher
John Wiley and Sons
Year
2003
Tongue
English
Weight
158 KB
Volume
42
Category
Article
ISSN
0044-8249

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✦ Synopsis


Dedicated to Professor G¸nther Jung on the occasion of his 65th birthday

Molecular recognition processes are predicted to become the basis of all advanced separation techniques. The investigation of intermolecular interactions in the interphase between a chromatographic support and a substrate dissolved in a mobile phase is the crucial condition for understanding chromatographic separation mechanisms and for the design of tailored stationary phases. In solution and also in suspension ligand±receptor interactions can be studied using methods of high-resolution (HR) NMR spectroscopy, for example by employing the nuclear Overhauser enhancement (NOE) 7.7 mmol). The solution was stirred 0.5 h at À78 8C and then another 5 h at RT. The resulting solution was added dropwise at À78 8C to a solution of ClP¼C(SiMe 3 ) 2 (1.74 g 7.7 mmol) in diethyl ether (30 mL). After stirring for 1 h at low temperature the solvent was removed under reduced pressure. The residue dissolved in n-hexane and then filtrated. After concentration of the filtrate solution 1 a precipitates in crystalline form as isomeric mixture rac/meso-1 a ¼ 4:1. MS (16 eV): m/z (%) ¼ 636 (8) [M] þ , 562 (66) [MÀSiMe 3 ] þ , 73 (100) [SiMe 3 ] þ ; 31