|Rink amide resin, or simply Rink resin, is used in solid phase peptide synthesis to prepare peptide amides utilizing Fmoc-protected amino acids. The peptide sequence is assembled under basic or neutral conditions on Rink amide resin, then the completed peptide is cleaved from the Rink resin under acid conditions. Typically the peptide is cleaved from Rink amide resin using 10% TFA in DCM. Stronger acids or higher concentrations of TFA sometimes cleaves some of the Rink linker from the polystyrene support and introduces colored impurities into the cleaved product. Rink amide MBHA resin is not as prone to these side reactions and is preffered by many peptide chemists. The following procedures are recommended for Rink amide resin and Rink amide MBHA resin.
Rink amide resin and Rink amide MBHA resin are available from AAPPTec.
|Rink Amide Resin
|Rink Amide MBHA Resin
For more information about Rink Amide Resin and other resins for peptide synthesis, click here.
Attaching the First Amino Acid to Rink amide Resin
|Preswell the Rink resin in DMF and deprotect with 20% piperidine/DMF for 20 to 30 minutes. Wash the resin thoroughly with DMF.
|Couple the appropriate C-terminal amino acid to the deprotected Rink amide resin using any of the standard coupling procedures. Remove a tiny amount of the resin and wash several times with DCM. Test for unreacted amine using the Kaiser test. If the test is positive, let the mixture stand for 30 minutes before repeating the test. Continue this procedure until the test is negative.
|Wash the amino acid Rink amide resin thoroughly with DMF, deprotect, and continue on with the synthesis.
Cleavage of the Peptide from Rink Amide Resin1
|Place the peptide-Rink resin in a round bottom flask and add 20% piperidine in DMF until the resin is just covered. Let the mixture stand for 30 minutes to remove the N-terminal Fmoc group.
|Transfer the deprotected peptide-Rink amide resin to a sintered glass funnel with fine porosity and apply vacuum. Wash the resin 3 times with DMF. Slurry the resin in DCM three times to remove the DMF.
|Slurry the peptide-Rink amide resin in 20% TFA in DCM (v/v) containing 3-5%(v/v) 1,3-dimethoxybenzene. Allow the mixture to stand at room temperature for 15 minutes. Filter and wash the resin with DCM.
|Combine the filtrates and add 8-10 times the volume of cold ether. If necessary, keep the mixture at 4 �C overnight to precipitate the peptide. Filter the peptide using a fine sintered glass funnel. Wash the crude peptide further with cold ether.
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|Based on procedures reported in Stathopoulos, P.; Papas, S.; Tsikaris, V. J. Pept. Sci. 2006, 12, 227-32.