Gram-positive bacterium resistant quaternary ammonium salt glycopeptides and medicinal applications thereof
A technology of antibacterial drugs and quaternary ammonium salt cations, applied in the direction of antibacterial drugs, glycopeptide components, peptides, etc., can solve problems such as irrational use of antibiotics, reduction of affinity between drugs and targets, and accelerated
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[0029] The invention provides a method for synthesizing the above-mentioned vancomycin quaternary ammonium salt derivatives, comprising: R 2 Nitrogen-containing groups and bromovaleric acid (bromoheptanoic acid, bromononanoic acid and bromodecanoic acid) are substituted to generate quaternary ammonium hydrochloride, and then condensed with NHS to generate active intermediates, and finally in alkaline
[0030] Under the conditions, the active intermediate is replaced by the sugar amino group of vancomycin to generate the above target compound. As shown in the reaction formula (1).
[0031]
[0032] Table of Target Compound Numbers
[0033]
[0034]
Embodiment 1
[0035] Embodiment 1: the synthesis of quaternary ammonium salt modified vancomycin derivative 1a
[0036] Dissolve 180mg (1.00mmol) of 5-bromovaleric acid in 5ml of pyridine, and reflux for 7h. TLC DCM:MEOH=1:1 monitored the disappearance of the starting material, and stopped heating. The reaction solution was rotary evaporated to a small volume, cooled, a solid precipitated, filtered, and the solid was washed with DCM several times to obtain 173 mg of a white powdery solid, with a yield of 96.1%. Weigh 100 mg (0.56 mmol) of the obtained solid compound, dissolve 96.7 mg (0.84 mmol) of NHS in DMF, add 141.3 mg (1.12 mmol) of DIC, and react at room temperature for 4 h. TLC monitored the completion of the raw material reaction, added 3-5 times the volume of diethyl ether to the reaction solution, discarded the solution to obtain an oil, purified by column chromatography to obtain 114.9 mg of the side chain compound, and the yield was 74%. Take a dry 10mL eggplant-shaped bottle,...
Embodiment 2
[0037] Example 2: For the synthesis of quaternary ammonium salt modified vancomycin derivative 1b, refer to the synthesis of 1a in Example 1.
[0038] White solid, yield 17%. 1 H NMR(400MHz,DMSO)δ:9.05(s,1H),8.61(s,1H),8.55(m,2H),,8.33(m,2H),8.24(s,1H),8.10(m,4H ),7.83(s,1H),7.54(s,1H),7.44(m,3H),7.29(m,2H),7.25(s,1H),7.20(d,J=7.4Hz,1H),7.12 (s,1H),6.75(s,1H),6.68(s,1H),6.65(s,1H),6.59(s,1H),6.41(s,1H),6.23(s,1H),5.97( s,1H),5.74(s,1H),5.57(s,1H),5.19(m,2H),5.14(s,2H),4.88(s,1H),4.69(s,1H),4.61(m ,2H),4.40(s,2H),4.24(s,1H),4.16(s,1H),3.22–3.55(m,6H),3.01(m,1H),2.83(s,2H),2.70( d,J=6.7Hz,2H),2.58(m,4H),2.20–2.00(m,6H),1.97(m,4H),1.80(m,3H),1.40(m,3H),1.50-1.30 (m,4H),1.02(m,2H),0.89(m,4H),0.78(m,9H).
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