Bis-fluoroquinolone oxadiazole urea derivatives containing N-methyl moxifloxacin as well as preparation method and application of derivatives
A technology of fluoroquinolone-based oxadiazuron and methylmoxifloxacin, which is applied in the field of new drug discovery and innovative drug synthesis
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[0048] The general method for the preparation of fluoroquinolone hydroxamic acid (1″~18″) is as follows: get the aforementioned fluoroquinolone carboxylic acid imidazolamide crude product (0.10 mol) and suspend it in 500mL pyridine, add hydroxylamine hydrochloride 7.0g~35.0g (0.1~0.5mol ), stirred and reacted in a water bath at 60-75°C for 8.0-24.0 hours, cooled to room temperature, collected the solid by filtration, washed the obtained solid with pyridine, dried in vacuum at 60-70°C, and dispersed in saturated sodium bicarbonate solution (500mL) again, 50 Stir in a water bath at ~65°C for 3 to 5 hours, collect the solid by filtration, wash with deionized water until the pH is 7.0, and dry to obtain the crude product. After recrystallization, analytically pure crystalline fluoroquinolone hydroxamic acid (1″-18″) was obtained.
[0049] General method for the preparation of target compound bis-fluoroquinolone-based oxadiazole derivatives containing N-methylmoxifloxacin: get 1.0 ...
Embodiment 1
[0053] 1-{2-[1-cyclopropyl-6-fluoro-8-methoxy-7-(1-methyl-octahydropyrrolo[3,4-b]pyridin-6-yl)-quinoline -4(1H)-keto-3-yl]-1,3,4-oxadiazol-5-yl}-3-[6-fluoro-7-(4-methylpiperazin-1-yl)- 8,1-(1,3-oxopropyl)-quinolin-4(1H)-one-3-yl]-urea (I-1), its chemical structural formula is:
[0054]
[0055] The preparation method of the bis-fluoroquinolone oxadiazuron of the present embodiment is: get ofloxacin hydroxamic acid (1 ") 1.0g (2.7 mmol) and suspend in 25mL acetonitrile, add carbonyldiimidazole (CDI) 0.79g (4.9mmol), stirring at room temperature until the material is dissolved. Then add 1.23g (2.7mmol) of N-methylmoxifloxacin C-3 oxadiazolamide II intermediate, and stir in a water bath at 55-60°C for 16 hours. Place overnight, filter The resulting solid was collected and washed with acetonitrile. The crude product was recrystallized from a mixed solvent of DMF-ethanol to obtain a light yellow crystal (I-1), with a yield of 56%, m.p.212-214°C. 1 H NMR (400MHz, DMSO-d 6 )δ: ...
Embodiment 2
[0057] (S)-1-{2-[1-cyclopropyl-6-fluoro-8-methoxy-7-(1-methyl-octahydropyrrolo[3,4-b]pyridin-6-yl )-quinoline-4(1H)-one-3-yl]-1,3,4-oxadiazol-5-yl}-3-[6-fluoro-7-(4-methylpiperazine-1 -yl)-8,1-(1,3-oxopropyl)-quinolin-4(1H)-one-3-yl]-urea (I-1), its chemical structural formula is:
[0058]
[0059] The preparation method of the bis-fluoroquinolone oxadiazuron of the present embodiment is: take levofloxacin hydroxamic acid (2″) 1.0g (2.7 mmol) and suspend in 25mL acetonitrile, add carbonyldiimidazole (CDI) 0.70g (4.3mmol ), stirred at room temperature until the material was dissolved. Then 1.23g (2.7mmol) of N-methylmoxifloxacin C-3 oxadiazole amine II intermediate was added, stirred in a water bath at 55-60°C for 10 hours. Placed overnight, and the resulting The solid was washed with acetonitrile. The crude product was recrystallized from ethanol to obtain a light yellow crystal (I-2), with a yield of 46%, m.p.206-208°C. 1 H NMR (400MHz, DMSO-d 6 )δ:11.64(brs,1H,NH), 9.5...
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