Pyrimidine-4 (3H)-ketone heterocyclic compound, preparation method thereof and application of pyrimidine-4 (3H)-ketone heterocyclic compound in medicine
A compound and heteroaromatic ring technology, applied to pyrimidine-4(3H)-one heterocyclic compound, its preparation and its application in medicine, can solve the problem of poor cell permeability, low bioavailability, selective Sexual problems, etc.
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Embodiment 1
[0107] (R)-5-((1H-pyrrolo[2,3-b]pyridin-4-yl)thio)-2-(1-amino-8-azaspiro[4.5]decane-8-yl )-3-methylpyrimidin-4(3H)-one
[0108]
[0109]
[0110] first step
[0111] 2-Chloro-5-iodopyrimidin-4(3H)-one
[0112] Dissolve 2,4-dichloro-5-iodopyrimidine 1a (8.0g, 29.1mmol) in tetrahydrofuran (100mL), add sodium hydroxide solution (1N, 45mL) at 0°C, and warm the reaction mixture to room temperature, stirring for 16 hours . The pH was adjusted to acidic with citric acid, and extracted with ethyl acetate (60 mL×3). The combined organic phases were washed with saturated brine (30mL×3), dried over anhydrous sodium sulfate, and precipitated under reduced pressure to obtain the target product 2-chloro-5-iodopyrimidin-4(3H)-one 1b (6.7g, solid), yield: 91%.
[0113] MS m / z(ESI):257[M+1]
[0114] second step
[0115] 2-Chloro-5-iodo-3-methylpyrimidin-4(3H)-one
[0116] 2-Chloro-5-iodopyrimidin-4(3H)-one 1b (5.6g, 21.7mmol) was dissolved in THF (100mL), methyl iodide (3.7g, 26m...
Embodiment 2
[0143] (R)-2-(1-amino-8-azaspiro[4.5]decane-8-yl)-3-methyl-5-((1-methyl-1H-pyrrolo[2,3- b] pyridin-4-yl)thio)pyrimidin-4(3H)-one
[0144]
[0145]
[0146] first step
[0147] 3-((1-Methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)thio)propanoic acid ethyl ester
[0148] To 4-bromo-1-methyl-1H-pyrrolo[2,3-b]pyridine 2a (200mg, 0.95mmol), ethyl 3-mercaptopropionate (255mg, 1.9mmol), N,N-diiso In a mixture of propylethylamine (368mg, 2.85mmol), 4,5-bis(diphenylphosphine)-9,9-dimethylxanthene (55mg, 0.095mmol) and dioxane (10mL) Tris(dibenzylideneacetone)dipalladium (87mg, 0.095mmol) was added, heated to 100°C under nitrogen protection, and reacted for 2 hours. Cool down to room temperature, add water (10 mL), and extract with ethyl acetate (20 mL×3). The organic phase was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, and the solvent was precipitated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl aceta...
Embodiment 3
[0164] (R)-5-((1H-indazol-4-yl)thio)-2-(1-amino-8-azaspiro[4.5]decane-8-yl)-3-methylpyrimidine- 4(3H)-keto
[0165]
[0166] first step
[0167] Ethyl 3-((1H-indazol-4-yl)thio)propionate
[0168] To a solution of 4-bromo-1H-indazole 3a (500 mg, 2.53 mmol) in dioxane (20 mL) was added ethyl 3-mercaptopropionate (680 mg, 5.06 mmol), N,N-diisopropylethyl Amine (979mg, 7.59mmol), tris(dibenzylideneacetone)dipalladium (231mg, 0.253mmol) and 4,5-bis(diphenylphosphine)-9,9-dimethylxanthene (219mg, 0.397 mmol). The reaction mixture was heated to 100°C under nitrogen for 2 hours. Cool down to room temperature, precipitate under reduced pressure, and purify the residue by silica gel column chromatography (ethyl acetate / petroleum ether=2.6 / 1) to obtain the target product 3-((1H-indazol-4-yl)thio)propionic acid Ethyl ester 3b (560 mg, solid), yield: 89%.
[0169] MS m / z(ESI):251[M+1]
[0170] second step
[0171] Sodium 1H-indazole-4-thiolate
[0172] To a solution of ethyl 3-...
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