By Lisa Bellavance English
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Extra info for Combinatorial Library
2. The volume of reaction vessels is adjustable by moving the syringe plunger. Consequently, different amounts of resin can be placed into individual syringes on the same block. Different sizes of syringes can also be attached to the same block; Manual Parallel Solid Phase Synthesis 3. 4. 5. 6. 7. 8. 9. 10. 57 they will always be filled, as the volume of the evacuated reaction vessel determines the volume of liquid introduced. It is not necessary to work with a fully loaded Domino Block. The remaining positions on a Domino Block can be closed using male Luer plugs.
2. 1. Resin Double-Loading, Attachment of Photolabile Linker, Encoding and Incorporation of RA Amine Synthons 1. 9 mmol) in 150 mL of 9:1 (v/v) DMF/DCM in a large shaking vessel. 4 mmol, 6 Eq). Shake the mixture for 16 h at 25°C. Drain the mixture and then wash the resin with 150 mL each of DMF (3×), MeOH (3×), and DCM (3×). Perform Nihydrin test for an aliquot of the resin; a negative result indicates complete coupling. 83 mmol, double loading, see Note 5). Place each portion into seven medium shaking vessels.
According to the tagging scheme for the 31 third-step synthons (Fig. 9), treat the resin in the 31 vessels with one or more of the T1–T5 tags. 5% of resin mass) in 100 µL of DCM. 5 mg/mL solution of [(CF3CO2)2Rh]2 in DCM. Shake the mixture at 25°C for 16 h. Drain the mixture and wash the resin with 5 mL each of DCM (4×), MeOH (2×), and DCM (4×). 3. Treat the resin in each of the 31 vessels with a unique RC Fmoc-amino acid synthon. 11 mmol). 32 mmol, 3 Eq). Shake the mixture at 25°C. Monitor the coupling reaction in the vessel using ninhydrin test to determine the level of the amine functionality remaining.