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13544276328
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Abbreviations used in this paper: BAL, backbone amide linker; AcOH, acetic acid; THF, tetrahydrofuran; DCM, dichloromethane; DMF, N,N-dimethylformamide; TFA, trifluoroacetic acid; and DIPEA, N,N-diisopropyllethylamine.
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3CN (from 8:2 to 3:7), with a flow rate of 2.0 mL/min and UV absorbance at 220 and 254 nm.
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13544261544
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2 in DCM solution, this solution (800 μmol, 0.585 mmol) was added slowly, and the reactor was shaken for 1.5 h at -10°C. The resin was washed with DCM (3 mL x 2), MeOH (3 mL x 2), and DCM (3 mL x 2) and then dried under vacuum for 3 h. DMF/thiourea 8 (1 mL/0.32 mmol) was added to the reactor, and the reactor was shaken for 12 h at 80°C. The resin was washed with DMF (3 mL x 2), MeOH (3 mL x 2), and DCM (3 mL x 2) and then dried under vacuum for 2 h. Finally, the resin was treated with 50% TFA/DCM for 30 min, from which the reaction mixture was filtered and concentrated within a Genevac model HT-4 evaporator.
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