I would very much like to be able to do disodium inosinate (IMP) and disodium guanylate (GMP) via GC. So far I've tried the chloroformates, phenylboronic acid for the ribose diol and then the chloroformate Pyridine+BSTFA+TMCS, Pyridine+MSTFA+TMCS, MSTFA+TMCS+ a few hours about 100 deg C and on column methylation with trimethylphenyl ammonium hydroxide. So far nothing has worked just empty chromatograms with traces of silyated impurities like glycerol or mid chain fatty acids.
I have Donald Knapp's book. It says Pyridine:BSTFA:TMCS 30:30:1 and either RT 30 min or 150degC. Several catelogs mention using Trimethylsilyl immidizaole which is strange as it only does hydroxyls and acids and won't do the amine on guanylate.
I am also concerned because to my knowledge nucleotides are not soluble in any organic solvents so after I evaporate it just sits there on the glass. Does anyone have a protocol that works?