Pyrimidine heterocyclic compound and its preparation method and application
A compound and drug technology, applied in the field of EGFR-mediated diseases, can solve the problems of increased affinity and decreased affinity of adenosine phosphate, and achieve the effect of good safety and toxicity parameters
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Embodiment 1
[0073] Example 1: 2-acrylamide-N-(2-(dimethylamino)ethyl)-5-methoxy-N-methyl-4-((4-(1-methyl-1H-ind Synthesis of Indol-3-yl)pyrimidin-2-yl)amino)aniline
[0074]
[0075] Step 1: Synthesis of methyl 5-methoxy-4-((4-(1-methyl-1H-indol-3-yl)pyrimidin-2-yl)amino)-2-nitrobenzoate:
[0076] Compound 3-(2-chloropyrimidin-4-yl)-1-methylindole (2.4g, 9.85mmol) and methyl 4-amino-5-methoxy-2-nitrobenzoate (2.67g , 11.82mmol) was added to the reaction flask, then 1,4-dioxane (20mL) was added, p-toluenesulfonic acid (2.03g, 11.82mmol) was added under stirring, and heated to 85°C for 48 hours, After the reaction was completed, it was cooled to room temperature, a solid was precipitated, filtered, the filter cake was washed with acetonitrile, and dried to obtain a yellow solid (4.0 g, yield: 93.7%). 1 H NMR (400MHz, CDCl 3 ):δ9.66(s,1H),8.44(d,J=4Hz,1H),8.21-8.19(m,1H), 8.17(s,1H),7.94(s,1H),7.44-7.41(m ,2H),7.28(s,1H),7.17(s,1H),4.06(s,3H),3.95(s,3H),3.93(s,3H).
[0077] Step 2: S...
Embodiment 2
[0085] Embodiment 2: N-(2-(dimethylamino)ethyl)-2-(3-(dimethylamino)propionylamino)-5-methoxy-N-methyl-4-(( Synthesis of 4-(1-methyl-1H-indol-3-yl)pyrimidin-2-yl)amino)benzamide
[0086]
[0087] Compound 2-acrylamide-N-(2-(dimethylamino)ethyl)-5-methoxy-N-methyl-4-((4-(1-methyl- 1H-indol-3-yl)pyrimidin-2-yl)amino)aniline (200mg, 0.38mmol) was added to the reaction flask, then ethanol (5mL) was added to dissolve, and 30% dimethylamine ethanol solution (2mL) was added under stirring ), stirred and reacted at room temperature for 30 minutes, after the completion of the reaction detected by TLC, concentrated, and purified by TLC to obtain the target compound as an off-white solid (100 mg, yield: 46.06%). 1 H NMR (400MHz, CDCl 3 )δ10.27(s,1H),9.16(s,1H),8.39(d,J=5.3Hz,2H),8.21(s,1H),7.80(s,1H),7.42–7.37(m,1H ),7.31(dd,J=8.9,5.2Hz,2H),7.17(d,J=5.3Hz,1H),6.77(s,1H),3.94(s,3H),3.87(s,3H),3.10 (s,3H),2.81(m,6H),2.55(s,6H),2.04(m,8H).MS(ESI)m / z573.32[M+H].
Embodiment 3
[0088]Example 3: N-(5-((4-(1-methyl-1H-indol-3-yl)pyrimidin-2-yl)amino)-2-(2,2,2-trifluoroacetyl )-4-(trifluoromethoxy) phenyl) acrylamide synthesis:
[0089]
[0090] Step 1: 2,2,2-Trifluoro-1-(4-((4-(1-methyl-1H-indol-3-yl)pyrimidin-2-yl)oxy)-2-nitro -Synthesis of 5-(trifluoromethoxy)phenyl)ethanone:
[0091] The compound 3-(2-chloropyrimidin-4-yl)-1-methylindole (1.5g, 6.16mmol) and 1-(4-amino-2-nitro-5-(trifluoromethoxy) Phenyl)-2,2,2-trifluoroethanone (1.96g, 6.16mmol) was added into the reaction flask, then 2-pentanol (100mL) was added, and p-toluenesulfonic acid monohydrate ( 1.27g, 7.39mmol), heated to 105°C for 2.5 hours, after the reaction, cooled to room temperature, precipitated solid, filtered, washed the filter cake with acetonitrile, dried to obtain a yellow solid (2.3g, yield: 71%). 1 H NMR (400MHz, CDCl 3 ):δ9.46(s,1H),8.56(d,1H),8.17(m,1H),7.59(m,1H),7.56(s,1H),7.50(s,1H),7.42-7.41( m,2H),7.19(s,1H),3.69(s,3H).
[0092] Step 2: 1-(2-Amino-4-((4-(1-me...
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