Hi,
I have synthesized an amide based compound that required purification via column chromatography using the solvent system DCM:MeOH:TEA (9.8:0.1:0.1). A clean fraction was obtained (approximately 1mg), however TEA is clearly observed in the 1H NMR. Is using the high vac is only way to remove the TEA? Are there any other methods that can be used for the tiny amount of sample obtained? The amide compound is soluble in DCM, MeOH, Chloroform and DMSO.
Thanks
Check https://www.chemicalforums.com/index.php?topic=50705.0
Hello Shivani,
Kindly check on this.
Article Methods for the analysis of galanthamine and its extraction ...
Dear Shivani,
many thanks for sharing this very interesting technical problem with the RG community. Due to the very small amount of your amide sample (1 mg), I would not suggest recrystallization or something like that. I assume that your amide product is a solid and not very volatile. Thus I would suggest to redissolve it in a few ml of DCM or chloroform and evaporate the solvent again under high vacuum, Triethylamine has a boiling point of 89 °C under normal pressure. This means that it is rather volatile and should evaporate together with the chosen solvent. Then dry the residue carefully under high vauum and run an NMR again. In the case that you dissolved the entire sample for the NMR measurement, it should be sufficient to just evaporate the solution in the NMR tube and dry the residue. This should remove the remaining triethylamine.
Good luck with this experiment and best wishes, Frank Edelmann
I totally agree with the suggestion of Frank T. Edelmann above. Best wishes
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