SYNTHESIS AND SPECTROMETRIC CHARACTERIZATION OF A TRUE DIOL BONDED PHASE

The syntheses of two types of diol bonded phases using a silanization/hydrosilation pathway are described. One product is similar to the phase produced by organosilanization but without the problem of potential side products and utilizes allyl glycidyl ether as the bonding olefin to the intermediate hydride. The second product is a ''true'' diol phase without any heteroatoms from the surface to the diol moiety and involves reacting 7-octene-1,2-diol with hydride silica. Both products can be obtained in good yield and the bonded phases can be characterized spectrometrically by diffuse reflectance IR Fourier transform and cross-polarization magic angle spinning NMR spectrometry. The only complication to this reaction scheme is bonding of the olefin diol to the silica surface via one of the alcohol groups (esterification). It appears that this is a problem when the original silica contains a significant number of unassociated silanol groups.