Substituted tetracycline compounds
A compound, tetracycline technology, applied in the direction of tetracycline active ingredients, preparation of organic compounds, drug combination, etc., can solve problems such as antibiotic resistance
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Embodiment 1
[0348] Embodiment 1: Synthesis of selected compounds of the present invention
[0349]
[0350] 7-iodo-shancycline (15.0g, 22.9mmol) and Pd(dppf) 2 Cl 2 (1.7g, 2.29mmol) and DMF (300ml) were mixed in a 1L round bottom two-neck flask to prepare the above compound. Na 2 CO 3 (7.2g, 68.2mmol) was dissolved in water (15ml), and then added to the reaction solution. 2-Fluoro-pyridine-5-boronic acid (6.4 g, 45.9 mmol) was dissolved in DMF (25 ml) and then also added to the reaction solution. Under argon atmosphere, the reaction mixture was stirred at 65°C (oil bath temperature), and the reaction was monitored by HPLC and LC / MS. The reaction was shown to be complete within 3 hours. Filter through celite and evaporate the solvent in vacuo. Redissolve in MeOH (30ml) and precipitate in MTBE (3L) to give a yellow precipitate. Filtration and vacuum drying overnight yielded 15 g of a yellow powder. The crude product (9 g, 17.8 mmol) was dissolved in TFA / trifluoromethanesulfonic ...
Embodiment 2
[0427] Embodiment 2: In vitro minimum inhibitory concentration (MIC) determination
[0428] The following experiments were used to determine the effect of tetracycline compounds on common bacteria. 2 mg of each compound was dissolved in 100 μl DMSO. This solution was then added to cation-adjusted Mueller Hinton Broth (CAMHB) at a final compound concentration of 200 μg / ml. The tetracycline compound solution was diluted to a volume of 50 µl and the test compound concentration was 0.098 µg / ml. Optical density (OD) measurements were performed on log-phase fresh broth cultures of the test strains. Dilute to a final cell density of 1 x 10 6 CFU / ml. When OD=1, the bacterial cell density of different genera should be approximately:
[0429] Escherichia coli (E.coli) 1×10 9 CFU / ml
[0430] Staphylococcus aureus (S.aureus) 5×10 8 CFU / ml
[0431] Enterococcus sp. 2.5×10 9 CFU / ml
[0432] Add 50 μl of bacterial cell suspension to each well of the microtiter plate. The final de...
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