Multivalent polyglycol (PEG) modifier for camptothecin and derivatives thereof and application of multivalent PEG modifier
A technology of modifiers and camptothecin, applied in the field of related drugs, can solve the problems of high proportion of invalid molecules and small effective drug loading
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Embodiment 1
[0049] Compound 1: [(Irinotecan-O-CO-CH 2 CH 2 -CO-) 2 -Lys-] 2 -PEG 20k Synthesis
[0050]
[0051] (1) Synthesis of irinotecan-20-succinic acid monoester (AA1)
[0052]
[0053] Irinotecan (5.86g, 10mmol), succinic anhydride (3g, 30mmol) and N,N-dimethyl-4-aminopyridine (DMAP, 300mg, 2.46mmol) were placed in a 100ml two-necked bottle under nitrogen protection , add 50ml of anhydrous pyridine. The reaction was stirred at room temperature for 12 hours, and the reaction progress was monitored by thin-layer chromatography until the reaction was complete. Concentrate under reduced pressure, pour the residue into ice water, place it, and filter to obtain a light yellow solid (5.28 g), with a yield of 77%.
[0054] ESI-MS m / z: 687.38 (M+H) +
[0055] 1 H-NMR (DMSO): δ 0.92 (t, 3H, CH 2 -CH 3 ), 2.13 (m, 7H), 2.49 (m, 2H), 2.7-2.8 (m, 13H), 5.27 (s, 2H), 5.47 (s, 2H), 7.05 (s, 1H), 7.50 (m, 2H), 8.07 (d, 1H), 8.55 (s, 1H), 12.26 (s, broad, 1H).
[0056] (2) Synth...
Embodiment 2
[0064] Compound 2: [(Camptothecin -O-CO-CH 2 CH 2 -CO-) 2 -Lys-] 2 -PEG 20k Synthesis
[0065]
[0066] (1) Synthesis of camptothecin-20-succinic acid monoester (BB1)
[0067]
[0068] Camptothecin (3.46g, 10mmol), succinic anhydride (3g, 30mmol) and N,N-dimethyl-4-aminopyridine (DMAP, 300mg, 2.46mmol) were placed in a 100ml two-necked bottle under nitrogen protection , add 50ml of anhydrous pyridine. The reaction was stirred at room temperature for 12 hours, and the reaction progress was monitored by thin-layer chromatography until the reaction was complete. Concentrate under reduced pressure, pour the residue into ice water, let it stand, and filter to obtain a light yellow solid (3.53 g), with a yield of 78.9%.
[0069] ESI-MS m / z: 449.79 (M+H) +
[0070] 1 H-NMR(DMSO): 2.13(m, 7H), 2.50(m, 2H), 2.7-2.8(m, 2H), 5.27(s, 2H), 5.50(s, 2H), 7.10(s, 1H) , 7.62 (m, 2H), 8.07 (d, 1H), 8.55 (s, 1H), 12.37 (s, broad, 1H).
[0071] (2) [(Camptothecin-O-CO-CH 2 CH ...
Embodiment 3
[0074] Embodiment 3: Determination of compound 2 blood drug concentration-time curve
[0075] 3 nude mice (20-25g) with a dose of 200mg / kg (equivalent to about 12.4mg / kg of camptothecin), injected compound 2 through the tail vein, and at different time points, the reversed-phase-high performance liquid chromatography Determination of the concentration of camptothecin in their plasma. The results showed that, 72 hours after administration, the total concentration of camptothecin in blood plasma could be maintained above 100ng / ml ( figure 1 ), indicating that multivalent polyethylene glycol-modified camptothecin can obtain long-acting effects.
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