Alkanosulfide-terminated oligomer-PEG modified amino-pyrazolo[3,4-d] pyrimidine derivative and application to non-small cell lung cancer resistance
A technology of alkyl and compound, applied in the field of pyrazolo[3,4-d]pyrimidine derivatives, which can solve the problems of high toxicity and side effects, low bioavailability, and low specificity
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Embodiment 1
[0044] The preparation of embodiment 1 compound 4
[0045]
[0046] Compound 1 (269mg, 1mmol) was dissolved in 1,4-dioxane / water (4:1) 150ml solution, and transferred to a 250ml round bottom flask, and then added (1.38g, 10mol) to the reaction solution Potassium carbonate, after stirring at room temperature for three minutes, add catalyst bis-diphenylphosphinoferrocene palladium chloride (73.1 mg, 0.1 mol), heat the reaction mixture to 100 ° C, detect the reaction by TLC, after the reaction is completed , first, after the reaction solution is cooled, add 50ml of distilled water, then transfer to a separatory funnel, add 100ml of dichloromethane to extract 3 times, combine the organic phases, add anhydrous sodium sulfate, spin dry the organic solvent, and dichloromethane / methanol (100:2.5) as eluent, separated and purified by silica gel column chromatography to obtain intermediate compound 2 (200 mg, 70%).
[0047] 1 H NMR (600MHz, DMSO-6d) δ9.83(s, 1H, HOAr), 8.28(s, 1H,...
Embodiment 2
[0054]
[0055] Synthesis of compound 2:
[0056] Compound 1 (269mg, 1mmol) was dissolved in 1,4-dioxane / water (4:1) 150ml solution, and transferred to a 250ml round bottom flask, and then added (1.38g, 10mol) to the reaction solution Potassium carbonate, after stirring at room temperature for three minutes, add catalyst bis-diphenylphosphinoferrocene palladium chloride (73.1 mg, 0.1 mol), heat the reaction mixture to 100 ° C, detect the reaction by TLC, after the reaction is completed , first, after the reaction solution is cooled, add 50ml of distilled water, then transfer to a separatory funnel, add 100ml of dichloromethane to extract 3 times, combine the organic phases, add anhydrous sodium sulfate, spin dry the organic solvent, and dichloromethane / methanol (100:2.5) as eluent, separated and purified by silica gel column chromatography to obtain intermediate compound 2 (200 mg, 70%).
[0057] 1 H NMR (600MHz, DMSO-6d) δ9.83(s, 1H, HO Ar), 8.28(s, 1H, CH), 6.97-7.83(m...
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