Chemical Biology 3OA3, September 2009 Page 44 1. Load your resin in DCM from last week back into the reaction tube. Use a Pasteur pipette, and gently transfer. Use more DCM to rinse the tube that the resin was stored in. 2. Remove the DCM by aspiration. 3. Re-swell the resin by washing with 1 mL of DMF twice. NOTE: recall the meaning of “wash” from last week). f. Final Fmoc removal and washing: 4. Remove the Fmoc group with 20% piperidine in DMF (as for steps 3-7 above, but remember half the quantities; remember not to let the resin go completely dry). 5. Wash the resin with 0.8 mL of DMF three times. 6. Wash the resin with 0.8 mL of methanol. 7. Wash the resin with 0.8 mL of DMF three times. 8. Wash the resin with 0.8 mL of DCM four times. g. Cleavage of product from the resin: [NOTE: do not start this part unless you can complete it at least to the end of step 13] 9. Make SURE the tap is closed, and stop the vacuum! Add 0.8 mL of 95% aqueous TFA to the resin. CAUTION: TFA fumes, smells bad, and is corrosive. WEAR GLOVES and handle
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This note was uploaded on 01/08/2012 for the course CHM 30A3 taught by Professor Ricktroendle during the Fall '11 term at UNF.