Phenylguanidine derivates containing pyrazolo pyrimidinone, medicament composition thereof as well as preparation method and application thereof
A technology of pyrazolopyrimidone and phenylguanidine, applied in the field of phenylguanidine derivatives, can solve the problems of photosensitivity, blurred vision, light vision and the like
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preparation example 1
[0164] 5-(5-Ethylamino-2-ethoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-7(6H)-one
[0165]
[0166] 5-(5-amino-2-ethoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-7(6H)-one (preparation method See Bioorg.Med.Chem.; 9; 7; 2001; 1895-1900.) (2.4g, 7.3mmol) was dissolved in 50ml80% acetonitrile aqueous solution, added 0.14g 5%Pd / C and 5g ammonium formate, nitrogen protection, Stir at room temperature for 20h. Palladium charcoal was filtered off, the solvent was evaporated to dryness and washed with 50ml CH 2 Cl 2 Dissolved, washed with water (50ml) and saturated brine (50ml) respectively, anhydrous Na 2 SO 4 Drying and concentration to dryness afforded a crude white solid. Purify by silica gel column chromatography (eluent: 10% petroleum ether-ethyl acetate) to obtain 2.4 g of the title compound with a yield of 92.1%. 1 H NMR (CDCl 3 )δ: 8.31(1H,d), 7.35(1H,dd), 7.13(1H,d), 4.27(3H,s), 4.21(2H,q), 4.01(2H,q), 2.92(2H,t ), 1.85 (2H, m), 1.36 (3H, ...
preparation example 2
[0168] 5-(5-Ethylamino-2-propoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-7(6H)-one
[0169]
[0170] According to the same method as Preparation Example 1, with 5-(5-amino-2-propoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidine-7 (6H)-Kone (for preparation see Bioorg. Med. Chem.; 9; 7; 2001; 1895-1900.) as starting material. The crude product was purified by silica gel column chromatography with a yield of 90.3%. 1 H NMR (CDCl 3 )δ: 8.31(1H,d), 7.35(1H,dd), 7.13(1H,d), 4.27(3H,s), 4.21(2H,t), 4.01(2H,q), 2.92(2H,t ), 2.03 (2H, m), 1.85 (2H, m), 1.36 (3H, t), 1.18 (3H, t), 1.02 (3H, t).
preparation example 3
[0172] 5-(5-Benzylamino-2-propoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-7(6H)-one
[0173]
[0174] 5-(5-amino-2-ethoxyphenyl)-1-methyl-3-propyl-1H-pyrazolo[4,3-d]pyrimidin-7(6H)-one (1.0g , 3.0mmol) was dissolved in 100ml methanol, slowly added dropwise benzaldehyde (0.33g, 3.1mmol), after TLC showed that the reaction ended, cooled with an ice bath, added NaBH in batches 4 (0.11 g, 3.1 mmol). After the reaction, the ethanol was evaporated to dryness, dissolved in dichloromethane (30ml), washed with water and saturated brine, anhydrous Na 2 SO 4 Dry, concentrate, and recrystallize from methanol / dichloromethane to obtain 1.05 g of the title compound, yield: 82.3%. 1 H NMR (CDCl 3 )δ: 7.55 (1H, d), 7.45-7.36 (6H, m), 7.20 (1H, d), 4.99 (2H, s), 4.16 (3H, s), 4.11 (2H, q), 2.75 (2H , t), 1.72 (2H, m), 1.31 (3H, t), 0.93 (3H, t).
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