I am new to peptide synthesis field. I am referring loading of of first amino acid on 2-chlorotrityl chloride resin. In procedure it is mentioned that after reaction wash it with DMF 4 x 1 min, what does it means, washed four times for 1 min or what else please explain. One more thing, if anybody have detail procedure for synthesis of 2-chlorotrityl chloride glycine (reaction of glycine with 2-chlorotrityl chloride resin), please send me file or please suggest any easy reference. I want procedure for conventional synthesis not the automated synthesis.
Add DMF, keep DMF with resin for 1min, then remove DMF, repeat 3 more times, total 4X. I think!
it means that you have to wash the resin four times and the duration of the washing is 1 minute each time. after washing every time remove all the solvent, and repeat the washing.
It should have been 4 x 1 mL and not 4 x 1 min. That means you can pass 1 mL DMF through the resin 4 times. The amount of DMF required depends upon what scale you are preparing the peptide.
Wash 4 times, hold the solvent for 1 min each time, don't wash directly..
1. Swell the resin in dry DCM for 15 to 20 min
2. Use 1.2 equivalents of the first amino acid (with respect to resin) dissolve in dry DCM (minimum amount) and 4 equivalents (with respect to the AA) of DIEA (N, N-Diisopropylethylamine).
3. Add it to the swelled resin.
4. Let it shake for 1 hour at room temp.
5. Wgen tge 1 hour finishes, add methanol (0.8ml per each g of the resin) to endcap any unreacted chloride of the CTC resin.
6. Wash 2 times with DMF and 2 times DCM, dry, there u go.
Make sure that the resin is in a good condition (if the chloride odor is strong and you can see a fumes coming up from the resin this means that the resin is in a good condition) otherwise, u need to activate the resin.
Cheers
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