Imidazodiazanaphthalene PI3K (phosphatidyl inositol 3 kinase) and mTOR (mammalian target of rapamycin) dual inhibitor
A kind of naphthalene and compound technology, applied in the field of imidazonaphthalene PI3K and mTOR dual inhibitors
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Embodiment 1
[0179] Example 1 8-(2-methoxypyridin-5-yl)-3-methyl-2-oxo-1-(piperidin-4-yl)-2,3-dihydroimidazo[4, 5-c][1,7] Preparation of naphthyridine (compound 1)
[0180] The preparation of embodiment 1-a (6-bromo-2-chloropyridine-3-amino) methylene malonate diethyl ester
[0181]
[0182]Add 20.7g (100mmol) of 6-bromo-3-amino-2-chloropyridine and 21.6g (100mmol) of diethyl ethoxymethylene malonate into 200mL of absolute ethanol, stir and reflux for 5 hours, and cool. A solid was precipitated and filtered to obtain 36.0 g of a white solid with a yield of 95.3%.
Embodiment 1-b
[0183] Example 1-b Preparation of 8-chloro-6-bromo-4-hydroxy[1,7]phthalazine-3-carboxylic acid ethyl ester
[0184]
[0185] 30.2g (80mmol) (6-bromo-2-chloropyridine-3-amino) diethyl methylene malonate was heated to reflux in 200mL diphenyl ether and stirred for 2 hours, then the reaction mixture was poured into petroleum ether, A yellow solid was precipitated, which was filtered and dried to obtain 24.5 g of the product, with a yield of 92.4%.
Embodiment 1-c
[0186] Example 1-c Preparation of 8-chloro-6-(2-methoxypyridin-5-yl)-4-hydroxy[1,7]phthalazine-3-carboxylic acid ethyl ester
[0187]
[0188] 16.6g (50mmol) 8-chloro-6-bromo-4-hydroxy [1,7] ethyl phthalazine-3-carboxylate, 9.18g (60mmol) 2-methoxypyridine-4-boronic acid, 1.6 g of bis(triphenylphosphine)palladium(II) dichloride and 50 mL of 1M Na 2 CO 3 The solution was added in 150mL DMF, stirred at room temperature for 2h, and the mixture was washed with saturated NaHCO 3 quenched with aqueous solution, then extracted with ethyl acetate, washed with brine, washed with Na 2 SO 4 After drying, filtering and evaporating to dryness under reduced pressure, 15.6 g of the product was obtained with a yield of 86.7%.
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