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- Posts: 1108
- Joined: Wed Dec 22, 2010 10:17 pm
- Location: Chicago
I have tried silylation many times and have never once had a successful reaction. I've tried it on inosinate and guanylate, acrylamide, now arginine. In each case when I inject I can see a huge intact silylation reagent peak (confirmed with the MSD) and some much smaller hydrolysis breakdown peaks some traces of silylated contaminants like glycerol or palmitic acid and a whole lot of nothing.
I've uses MSTFA, BSTFA, +TMCS and TMSI.
I've trield acetonitrile, pyridine and DMSO as solvents.
I typically heat to 70 deg C for 30 minutes to overnight.
I do the reaction in an autosampler tube.
same results. How can a confirmed active reagent and anayte go into the same vial and not react?