Quindoline derivative, medicine composition thereof, preparation method and application
A derivative and quinoline technology, applied in the field of quinoline derivatives, can solve the problems of large differences in the activity of compounds, no structure-activity relationship, unsatisfactory and other problems
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Embodiment 1
[0064] Example 1: 9-{difluoro[6-(1-methyl-1H-pyrazol-4-yl)-[1,2,4]triazolo[4,3-b]pyridazine-3- Synthesis of base]methyl}-8-fluoro-4-methyl-2H-[1,4]oxazizo[3,2-c]quinolin-3(4H)-one
[0065] The synthetic route is as follows:
[0066]
[0067] Step 1: Preparation of 3-amino-6-bromo-7-fluoro-quinoline-4-ol (HJ-1)
[0068] Add compound 6-bromo-7-fluoro-3-nitroquinoline-4-ol (2.5g, 9.0mmol) and methanol (15ml) in 100ml one-necked flask, add hydrazine hydrate (2.7g, 46.5ml) under ice bath mmol) and Raney nickel (0.45mmol), stirred at room temperature until the end of the reaction. The reaction solution was filtered, the filter cake was washed three times with methanol, and the organic phase was spin-dried to obtain 2.20 g of compound 3-amino-6-bromo-7-fluoro-quinoline-4-ol (HJ-1), with a yield of 95% ;MSm / z(ESI):258.89([M+l] + ).
[0069] Step 2: Preparation of 9-bromo-8-fluoro-2H-[1,4]oxazino[3,2-c]quinolin-3(4H)-one (HJ-2)
[0070] Add (HJ-1) (2.10g, 8.8mmol) prepared in ...
Embodiment 2
[0082] Example 2: 8-fluoro-4-methyl-9-{[6-(1-methyl-1H-pyrazol-4-yl)-[1,2,4]triazolo[4,3- b] Pyridazin-3-yl]sulfanyl}-2H-[1,4]oxazizo[3,2-c]quinolin-3(4H)-one
[0083] The synthetic route is as follows:
[0084]
[0085] Step 1: Preparation of 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine (HJ-8)
[0086] Add dioxane (67ml) and water (27ml) in the three-necked flask of 250ml as solvent, then add successively 3,6-dichloropyridazine (2.68g, 18mmol), potassium carbonate (6.0g, 43.5mmol), 1-methylpyrazole-4-boronic acid pinacol ester (2.99g, 14.4mmol), [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride (0.7g, 0.96mmol ), after replacing with nitrogen, the temperature was raised to 80°C. After reacting for 10 hours, the reaction solution was concentrated and separated by column chromatography to obtain 1.96 g of light yellow solid 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine (HJ-8) , yield 70%; MSm / z (ESI): 195.12 ([M+l] + ).
[0087] Step 2: Preparation of 3-h...
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