Cyclic iminopyrimidine derivatives as kinase inhibitors
A technology of derivatives and solvates, applied in the field of cyclic iminopyrimidine derivatives as kinase inhibitors, can solve the problems of being unsuitable for brain tumors or cancer, low penetration into cell membranes, and into the brain
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Embodiment 1
[0259] Example 1: Preparation of N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)phenyl)propane-1- Sulfonamide (Compound 1)
[0260] plan 1
[0261]
[0262] Step 1: Synthesis of 6-methoxyquinazolin-4(3H)-one
[0263] A mixture of 2-amino-5-methoxybenzoic acid (10.0 g, 59.9 mmol), formamidine acetate (12.3 g, 119 mmol) in 80 mL of 2-methoxyethanol was heated at 125°C for 18 hours. After cooling to room temperature, the precipitate was collected by filtration, washed twice with 2-methoxyethanol, and dried in vacuo to provide 6-methoxyquinazolin-4(3H)-one (9.1 g, 87% yield Rate).
[0264] Step 2: Synthetic 4-chloro-6-methoxyquinazoline
[0265] 6-Methoxyquinazolin-4(3H)-one (3.0g, 17.0mmol) in POCl 3 (30 mL) and the solution was stirred overnight at 120°C. The mixture was then cooled to room temperature and evaporated. The residue was purified by silica gel column chromatography (PE / EtOAc from 10:1 to 5:1, v / v) to give 4-chloro-6-methoxyquinazoline (3.0 g, ...
Embodiment 2
[0276] Example 2: Preparation of N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)phenyl)-N-methyl Propane-1-sulfonamide (Compound 2)
[0277] Scenario 2
[0278]
[0279] Synthesis of N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)phenyl)-N-methylpropane-1 -sulfonamide
[0280] 0°C, NaH (60% in mineral oil, 16.0 mg, 0.39 mmol) was slowly added to N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazole In a solution of olin-9-yl)oxy)phenyl)propane-1-sulfonamide (80mg, 0.20mmol) in DMF (10.0mL). The reaction mixture was washed with N 2 Degas and stir at room temperature for 60 minutes. Iodomethane (43 mg, 0.30 mmol) was then added, and the mixture was stirred at room temperature overnight under nitrogen. The resulting mixture was evaporated and the residue was purified by flash column chromatography (ACN / H 2 O), to give N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)phenyl)-N-methyl Propane-1-sulfonamide (30 mg, 35% yield) as a white so...
Embodiment 3
[0281] Example 3: Preparation of N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)-4-fluorophenyl) Propane-1-sulfonamide (Compound 3)
[0282] Option 3
[0283]
[0284] Step 1: Synthesis of 2-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)-3,6-difluorobenzonitrile
[0285] 0 °C, NaH (60% in mineral oil, 111 mg, 2.78 mmol) was slowly added to 2,3-dihydroimidazo[1,2-c]quinazolin-9-ol (400 mg, 2.14 mmol) in DMF (20mL) solution. The reaction mixture was washed with N 2 Degas and stir at room temperature for 60 minutes. Then 2,3,6-trifluorobenzonitrile (37.0 mg, 2.35 mmol) was added, and the mixture was stirred at 80° C. for 1 hour. The resulting mixture was evaporated and the residue was purified by silica gel column chromatography (DCM / MeOH from 100:1 to 30:1, v / v) to give 2-((2,3-dihydroimidazo[1,2- c] quinazolin-9-yl)oxy)-3,6-difluorobenzonitrile (200 mg, 29% yield).
[0286] Step 2: Synthesis of N-(2-cyano-3-((2,3-dihydroimidazo[1,2-c]quinazolin-9-yl)oxy)...
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