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Resin cleavage (revision 2)

Old revision·20:17, 12 Aug 2024·FiveOhThreeB

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Resin cleavage
Reagent, Fmoc chemistryTrifluoroacetic acid with scavengers
SimultaneousSide-chain deprotection
IsolationPrecipitation into cold ether
Analytical method infobox · conventions

Resin cleavage is the step that releases an assembled peptide from the solid support. In Fmoc chemistry it also removes the acid-labile side-chain protecting groups, so a single treatment with concentrated trifluoroacetic acid accomplishes both.[1]

The removed protecting groups generate reactive carbocations, which will alkylate electron-rich side chains — tryptophan, methionine, cysteine and tyrosine — unless captured. Scavengers are included in the cleavage cocktail for that purpose, and their selection depends on which residues the sequence contains.[1]

Cocktails and scavengers

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A typical cocktail is trifluoroacetic acid with a few per cent each of water, triisopropylsilane and, where cysteine or methionine is present, a thiol scavenger. Water and silane trap the tert-butyl and trityl cations; thiols address the more persistent species.[1]

Time and temperature are the other variables. Arginine's sulfonyl protecting groups are the slowest to remove, so a peptide rich in arginine requires longer treatment — during which more sensitive residues are exposed to acid for longer.

References

  1. ^ a b c Behrendt R, White P, Offer J. "Advances in Fmoc solid-phase peptide synthesis." Journal of Peptide Science 22(1):4–27 (2016). PMID 26785684.