Peptides 1 to 5 (Fig. 1) were synthesized by microwave-assisted standard Boc-SPPS method. Briefly, deprotection of the Boc group was performed twice (1× 2 min and 1× 3 min) with neat TFA, and double coupling of amino acids was applied (1× 5 min and 1× 10 min, 20 W, 70°C). Amino acids were activated by DIPEA and HATU. Peptides were cleaved by anhydrous hydrogen fluoride with addition of p-cresol as a scavenger. Compounds 1 to 5 were purified by RP-HPLC.

Compound 1. Yield: 34%. Molecular weight: 4823.63. ESI-MS [M + 3H]3+ m/z 1608.6 (calc. 1608.9), [M + 4H]4+ m/z 1206.8 (calc. 1206.9), [M + 5H]5+ m/z 965.8 (calc. 965.7), [M + 6H]6+ m/z 804.9 (calc. 804.9), [M + 7H]7+ m/z 690.1 (calc. 690.1), [M + 8H]8+ m/z 603.9 (calc. 604.0), [M + 9H]9+ m/z 537.0 (calc. 537.0). tR = 19.1 min (0 to 100% solvent B; C4 column); purity ≥ 99%.

Compound 2. Yield: 23%. Molecular weight: 5814.96. ESI-MS [M + 3H]3+ m/z 1938.6 (calc. 1939.3), [M + 4H]4+ m/z 1455.0 (calc. 1454.7), [M + 5H]5+ m/z 1164.0 (calc. 1164.0), [M + 6H]6+ m/z 969.9 (calc. 970.1), [M + 7H]7+ m/z 831.5 (calc. 831.7), [M + 8H]8+ m/z 728.0 (calc. 727.9). tR = 24.1 min (0 to 100% solvent B; C4 column); purity ≥ 99%.

Compound 3. Yield: 28%. Molecular weight: 6295.40. ESI-MS [M + 4H]4+ m/z 1574.7 (calc. 1574.9), [M + 5H]5+ m/z 1260.0 (calc. 1260.0), [M + 6H]6+ m/z 1050.3 (calc. 1050.2), [M + 7H]7+ m/z 900.4 (calc. 900.3), [M + 8H]8+ m/z 788.0 (calc. 787.9), [M + 9H]9+ m/z 700.7 (calc. 700.5). tR = 24.5 min (0 to 100% solvent B; C4 column); purity ≥ 99%.

Compound 4. Yield: 28%. Molecular weight: 5955.23. ESI-MS [M + 3H]3+ m/z 1985.2 (calc. 1986.1), [M + 4H]4+ m/z 1489.6 (calc. 1489.8), [M + 5H]5+ m/z 1192.0 (calc. 1192.0), [M + 6H]6+ m/z 993.5 (calc. 993.5), [M + 7H]7+ m/z 851.8 (calc. 851.7), [M + 8H]8+ m/z 745.4 (calc. 745.4). tR = 25.6 min (0 to 100% solvent B; C4 column); purity ≥ 99%.

Compound 5. Yield: 26%. Molecular weight: 6521.03. ESI-MS [M + 4H]4+ m/z 1631.8 (calc. 1631.3), [M + 5H]5+ m/z 1305.6 (calc. 1305.2), [M + 6H]6+ m/z 1088.0 (calc. 1087.8), [M + 7H]7+ m/z 932.9 (calc. 932.6), [M + 8H]8+ m/z 816.3 (calc. 816.1), [M + 9H]9+ m/z 725.6 (calc. 725.6). tR = 30.9 min (0 to 100% solvent B; C4 column); purity ≥ 99%.

注意:以上内容是从某篇研究文章中自动提取的,可能无法正确显示。



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