A kind of multi-armed pegized oritavancin derivative and its preparation
A technology of oritavancin and its derivatives, applied in the application field of multi-armed PEGylated oritavancin derivatives and their preparation, preparation and treatment of acute bacterial skin and skin structure infections, capable of solving To avoid problems such as limited quantity, to achieve the effects of convenient quality control, good drug activity in vivo and in vitro, and reduced toxic and side effects
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Embodiment 1
[0028] (1) Preparation of 4-Arm-PEG24-GA-II
[0029] Dissolve 10mmol of 4-Arm-PEG24-OH-I in 100ml of DMF, add 11mmol of adipic anhydride and 10mmol of DMAP at room temperature, and then stir at 100°C for 10h. After the reaction was completed, the solution was distilled off under reduced pressure to obtain a crude product. The crude product was purified by chromatography to obtain 4-Arm-PEG24-GA-II. Yield: 90%. NMR data are as follows: 1H NMR (400MHz, CDCl3) δ4.26(s,2H),3.66(m,96H),2.86(s,2H),2.74(s,2H),2.52(s,2H), 2.09( s,2H).
[0030] (2) Preparation of 4Arm-PEG24-oritavancin-II
[0031] Dissolve 10mmol of 4-Arm-PEGm-GA-II in 50ml of N,N-dimethylformamide, add 10mmol of DIC and 10mmol of 4-PPY, and stir at 25°C for 2h. 80 mmol of oritavancin was added to the reaction, and the reaction was carried out at 30°C for 12 hours. After the completion of the oritavancin reaction as detected by TLC tracking, 4Arm-PEG24-oritavancin-II was obtained by recrystallization and chromato...
Embodiment 2
[0033] (1) Preparation of 4-Arm-PEG124-GA-II
[0034] Dissolve 10mmol of 4-Arm-PEG124-OH-I in 100ml of DMF, add 11mmol of adipic anhydride and 10mmol of DMAP at room temperature, and then stir at 100°C for 8h. After the reaction was completed, the solution was distilled off under reduced pressure to obtain a crude product. The crude product was purified by chromatography to obtain (4or 6or 8)-Arm-PEGm-GA-II. Yield: 90%. NMR data are as follows: 1H NMR (400MHz, CDCl3) δ4.26(s,2H),3.66(m,496H),2.86(s,2H),2.74(s,2H),2.52(s,2H),2.09( s,2H).
[0035] (2) Preparation of 4Arm-PEG124-oritavancin-II
[0036] Dissolve 10mmol of 4-Arm-PEG24-GA-II in 50ml of N,N-dimethylformamide, add 10mmol of DIC and 10mmol of 4-PPY, and stir at 25°C for 2h. 80 mmol of oritavancin was added to the reaction, and the reaction was carried out at 30°C for 12 hours. After TLC tracking detection oritavancin reaction was complete, 4Arm-PEG124-oritavancin-II was obtained by recrystallization and chromatog...
Embodiment 3
[0038] (1) Preparation of 4-Arm-PEG240-GA-II
[0039] Dissolve 10mmol of 4-Arm-PEG240-OH-I in 100ml of DMF, add 11mmol of adipic anhydride and 10mmol of DMAP at room temperature, and then stir at 120°C for 10h. After the reaction was completed, the solution was distilled off under reduced pressure to obtain a crude product. The crude product was purified by chromatography to obtain 4-Arm-PEG240-GA-II. Yield: 90%. NMR data are as follows: 1H NMR (400MHz, CDCl3) δ4.26(s, 2H), 3.66(m, 960H), 2.86(s, 2H), 2.74(s, 2H), 2.52(s, 2H), 2.09( s,2H).
[0040] (2) Preparation of 4Arm-PEG240-oritavancin-II
[0041] Dissolve 10mmol of 4-Arm-PEG240-GA-II in 50ml of N,N-dimethylformamide, add 10mmol of DIC and 10mmol of 4-PPY, and stir at 25°C for 2h. 80 mmol of oritavancin was added to the reaction, and the reaction was carried out at 30°C for 12 hours. After TLC tracking detection oritavancin reaction was complete, 4Arm-PEG240-oritavancin-II was obtained by recrystallization and chromat...
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