Heterocyclic compound serving as protein kinase inhibitor as well as preparation method and application thereof
A technology of compounds and solvates, applied in the field of protein kinase inhibitors, can solve the problems of uncontrolled cell growth, loss of cell growth, cancer, etc.
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Embodiment 2
[0131] Example 2: 5-(2-fluoro-4-iodophenylamino)-N-(2-hydroxyethoxy)-9-methylfuro[3,2-c]imidazo[1,5- a] pyridine-6-carboxamide
[0132]
[0133] Step 1: Synthesis of ethyl 2-(2-ethoxy-2-oxoethyl)-4-methylfuran-3-carboxylate
[0134]
[0135] The title compound was prepared according to J. Am. Chem. Soc, 1985, 107, 2196-2198... l H-NMR (400MHz, CDCl 3 )δ7.13(s,1H),4.28(q,J=7.2Hz,2H),4.18(q,J=6.8Hz,2H),4.01(s,2H),2.17(s,3H),1.34( t,J=6.8Hz,3H),1.26 (t,J=7.2Hz,3H).
[0136] Step 2: 6-(2-Fluoro-4-iodophenylamino)-3-methyl-4-oxo-4,5-dihydrofuro[3,2-c]pyridine-7-carboxylic acid ethyl Synthesis of esters
[0137]
[0138] Ethyl 2-(2-ethoxy-2-oxoethyl)-4-methylfuran-3-carboxylate (6.0g, 24.97mmol 1.0eq) in anhydrous THF (50ml ) to the stirred solution was added NaH (1.1 g, 27.47 mmol 1.1 eq..60%) in portions. Then, 2-fluoro-N-(iminomethylene)-4-iodoaniline (7.2 g, 27.47 mmol 1.1 eq.) was added slowly over 1 hour using a dropping funnel, and then the mixture was stirred...
Embodiment 3
[0163] Example 3: 5-(2-fluoro-4-iodophenylamino)-N-(2-hydroxyethoxy)imidazo[1,5-a]thieno[3,2-c]pyridine-6 -Formamide
[0164]
[0165] Step 1: Synthesis of methyl 2-(2-methoxy-2-oxoethyl)thiophene-3-carboxylate
[0166]
[0167] The title compound was prepared according to WO 2005087779. lH NMR (400MHz, DMSO-D6). δ7.46 (d, J = 5.6Hz, 1H), 7.36 (d, J = 5.6Hz, 1H), 4.21 (s, 2H), 3.73 (s, 3H), 3.61 (s, 3H).
[0168] Step 2: Synthesis of methyl 6-(2-fluoro-4-iodophenylamino)-4-oxo-4,5-dihydrothieno[3,2-c]pyridine-7-carboxylate
[0169]
[0170] Into a stirred solution of methyl 2-(2-methoxy-2-oxoethyl)thiophene-3-carboxylate (5.0 g, 23.34 mmol 1.0 eq) in anhydrous THF (50 mL) at 0°C NaH (1.03g, 25.67mmol 1.1eq..60%) was added in batches. Then, 2-fluoro-N-(iminomethylene)-4-iodoaniline (6.73 g, 25.67 mmol 1.1 eq.) was added slowly over 1 hour using a dropping funnel, and then the mixture was stirred at room temperature overnight. After adding water and ethyl acetate,...
Embodiment 4
[0195] Example 4: 5-(2-fluoro-4-iodophenylamino)-N-(2-hydroxyethoxy)imidazo[1,5-a]thiazolo[4,5-c]pyridine-4 -Formamide
[0196]
[0197] Step 1: Synthesis of methyl 5-(2-methoxy-2-oxoethyl)thiazole-4-carboxylate
[0198]
[0199] The title compound was prepared according to Bioorganic & Medicinal Chemistry Letters, 2008, 18(6), 2206-2210... 1H NMR (400MHz, CDC13): δ8.75(s, 1H), 4.38(s, 2H), 3.96(s, 3H), 3.78(s, 3H).
[0200] Step 2: Synthesis of methyl 6-(2-2-fluoro-4-iodophenylamino)-4-oxo-4,5-dihydrothiazolo[4,5-c]pyridine-7-carboxylate
[0201]
[0202] To a stirred solution of methyl 5-(2-methoxy-2-oxoethyl)thiazole-4-carboxylate (5.0 g, 23.23 mmol 1.0 eq) in anhydrous THF (50 mL) at 0°C NaH (1.02 g, 25.55 mmol 1.1 eq..60%) was added in portions. Then, 2-fluoro-N-(iminomethylene)-4-iodoaniline (6.70 g, 25.55 mmol 1.1 eq.) was added slowly over 1 hour using a dropping funnel, and then the mixture was stirred at room temperature overnight. After adding water an...
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