The reactions were terminated by the addition of 1 N H2SO4, and the optical densities were measured at 450 nm using an ELISA plate reader (Molecular Device, Sunnyvale, CA)
The reactions were terminated by the addition of 1 N H2SO4, and the optical densities were measured at 450 nm using an ELISA plate reader (Molecular Device, Sunnyvale, CA). inhibit Plk1 PBD. = 745.8 [M+H]+. Cyclic peptide, PL-2. Synthesis on 0.058 mmol scale. Purity of crude product 42% (C18 RP-HPLC). Yield after purification: 9 mg, 22%; white powder; RP-HPLC = 702.1 [M ? 1]. Cyclic peptide, PL-3. Synthesis on 0.062 mmol scale. Purity of crude product 11% (C18 RP-HPLC). Yield after purification: 2 mg, 5%; white powder; RP-HPLC = 647.52 [M+H]+. 3.6. Peptide synthesis by thioether-bridged GSK4716 bond formation As mentioned above, using Fmoc protection strategy, the linear side-chain guarded peptide was synthesized around the Rink amide resin (0.61 mmol/g) coupled with the respective amino acids, and the Fmoc group in the N-terminal of the resin-bound protected peptide was removed with 20% piperidine/DMF. Then, the resin-bound guarded peptide was N-terminally bromoacetylated by (BrCH2CO)2O which was prepared by mixing 10.0 equiv of BrCH2COOH and 5.0 equiv of DIC for 3 h at rt. The peptide (0.061 mmol) was cleaved from the resin and dissolved in 10 mL of water/CH3CN (1:1) mixture followed by the dropwise addition of triethylamine to adjust the pH 8C9, repeatedly. Under the basic conditions the N= 750.26 [M+H]+. Cyclic peptide, PL-5. Synthesis on 0.061 Rabbit Polyclonal to ELOVL1 mmol scale. Purity of crude product 23% (C18 RP-HPLC). Yield after purification: 5.2 mg, 11%; white powder; RP-HPLC = 775.67 [M]. Cyclic peptomer, PL-6. Synthesis on 0.061 mmol scale. Purity of crude product 44% (C18 RP-HPLC). Yield after purification: 11.2 mg, 21%; white powder; RP-HPLC = 874.91 [M+H]+. Cyclic peptomer, PL-7. Synthesis on 0.055 mmol scale. Purity of crude product 21% (C18 RP-HPLC). Yield after purification: 5.2 mg, 11%; white powder; RP-HPLC = 868.51 [M+H]+. Cyclic peptomer, PL-8. Synthesis on 0.061 mmol scale. Purity of crude product 30.1% (C18 RP-HPLC). Yield after GSK4716 purification: 7.2 mg, 14%; white powder; RP-HPLC = 838.67 [M ? 1]. Cyclic peptomer, PL-9. Synthesis on 0.061 mmol scale. Purity of crude product 17.5% (C18 RP-HPLC). Yield after purification: 4 mg, 8%; white powder; RP-HPLC = 826.62 [M+H]+. Cyclic peptomer, PL-10. Synthesis on 0.062 mmol scale. Purity of crude product 53.6% (C18 RP-HPLC). Yield after purification: 13 mg, 25%; white powder; RP-HPLC = 844.72 [M+H]+. Cyclic peptomer, PL-21. Synthesis on 0.041 mmol scale. Purity of crude product 31% (C18 RP-HPLC). Yield after purification: 2.9 mg, 8%; white powder; RP-HPLC = 870.18 [M+H]+. Cyclic peptomer, PL-22. Synthesis on 0.036 mmol scale. Purity of crude product 14% (C18 RP-HPLC). Yield after purification: 1 mg, 3%; white powder; RP-HPLC = 872.20 [M+H]+. Cyclic peptomer, PL-23. Synthesis on 0.061 mmol scale. Purity of crude product 13% (C18 RP-HPLC). Yield after purification: 2.5 mg, 5%; white powder; RP-HPLC = 877.31 [M ? 1]. Cyclic peptomer, PL-28. Synthesis on 0.061 mmol scale. Purity of crude product 7% (C18 RP-HPLC). Yield after purification: 3.3 mg, 6%; white powder; RP-HPLC = 863.30 [M ? 1]. Cyclic peptomer, PL-29. Synthesis on 0.061 mmol scale. Purity of crude product 10% (C18 RP-HPLC). Yield after purification: 0.5 mg, 1%; white powder; RP-HPLC = 766.30 [M+H]+. Cyclic peptomer, PL-30. Synthesis on 0.061 mmol scale. Purity of crude product 13% (C18 RP-HPLC). Yield after purification: 4.7 mg, 9%; white powder; RP-HPLC = 877.31 [M1]. 3.7. Synthesis of (= 7.2 Hz, 2H), 3.39 (s, 2H), 2.41 (d, = 6.7 Hz, 2H), 1.74 (quintet, 1H), 1.56 (br s, 1H), 1.28 (t, = 7.2 Hz, 3H), 0.93 (d, = 6.7 Hz, 6H). 3.7.2. = 6.0 Hz, 2H), 4.16C4.25 (m, 1H), 3.87, 3.99 (two s, 2H), 2.93, 3.13 (two d, = 7.5 Hz, 2H), 1.61, 1.82 (two septets, 1H), GSK4716 0.72, 0.87 (two doublets, = 6.8 Hz 6H). All data were in agreement with the reported values.18 3.7.3. Thioether-bridged cyclic peptomers having double peptoid Cyclic peptomer, PL-11. Synthesis on 0.041 mmol scale. Purity of crude product 21.6% (C18 RP-HPLC). Yield after purification: 2.2 mg, 8%; white powder; RP-HPLC = 679.57 [M+H]+. Cyclic peptomer, PL-12. Synthesis on 0.061 mmol.