A kind of synthetic method of metronidazole-sulfonamide derivative
A derivative, the technology of metronidazole, is applied in the field of synthesis of a class of metronidazole-sulfonamide derivatives, which can solve the problems of no bactericidal effect, easy drug resistance, and limited application range
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Embodiment 1
[0013] Example 1: Preparation of 3-(2-(2-methyl-5-nitro-1-imidazole)ethoxy)-benzaldehyde (compound 3)
[0014]
[0015] Under stirring, 3-(2-(2-methyl-5-nitro-1-imidazole)ethoxy)-4-methylbenzenesulfonate (4.0g, 12.1mmol), DMF (150mL) , anhydrous potassium carbonate (8.0g, 58mmol), 3-hydroxybenzaldehyde (1.9g, 15.7mmol) were added in a 250mL round-bottomed flask, and stirred at a constant temperature of 80°C for 20 hours (TLC followed the reaction; developer: V 二氯甲烷 :V 乙酸乙酯 =2:1), the reaction solution was poured into distilled water (300mL), extracted with ethyl acetate, the organic layers were combined, dried over anhydrous magnesium sulfate, the solvent was removed under reduced pressure, column chromatography (eluent: V 二氯甲烷 :V 乙酸乙酯 =2:1) to obtain 1.7 g of light yellow solid. Yield 51.3%. m.p.41~43°C; 1 H NMR (DMSO-d 6 , 300MHz) δ: 9.95(s, 1H, CHO), 7.91(s, 1H, CH), 7.96(s, 1H, ArH), 7.47~7.05(m, 3H, ArH), 4.75(t, J=4.7 Hz, 2H, -CH 2 ), 4.39 (t, J=5.0Hz, 2H, -CH...
Embodiment 2
[0016] Example 2: Preparation of 4-(3-(2-(2-methyl-5-nitro-1-imidazole)ethoxy)-benzaldehyde)sulfonamide (compound 4)
[0017]
[0018] The compound 4-(2-(2-methyl-5-nitro-1-imidazole)ethoxy)-benzaldehyde (0.25g, 0.78mmol), ethanol (15mL), sulfonamide (0.22g , 0.78mmol), glacial acetic acid (0.3mL) was added to a 25mL round bottom flask, heated at 50°C for 8h (reaction monitored by TLC; developer: V 二氯甲烷 :V 乙酸乙酯 =1:1), after the reaction was completed, part of the solvent was removed under reduced pressure, a small amount of distilled water was added, filtered, and dried to obtain 0.21 g of an orange-yellow solid, with a yield of 66.5%. m.p.195-197°C; 1 H NMR (DMSO-d 6 , 300MHz) δ: 8.52(s, 1H, CH), 8.03(s, 1H, CH), 7.88~7.03(m, 8H, ArH), 7.04(s, 1H, NH), 7.02(s, 1H, NH ), 4.75(t, J=4.7Hz, 2H, -CH 2 ), 4.39 (t, J=5.0Hz, 2H, -CH 2 ), 2.48(s, 3H, CH 3 ).
Embodiment 3
[0019] Example 3: Preparation of 4-(3-(2-(2-methyl-5-nitro-1-imidazole)ethoxy)-benzaldehyde)sulfathiazole (compound 5)
[0020]
[0021] The preparation method is the same as that in Example 2. Sulfathiazole is used instead of sulfonamide to obtain the orange-yellow target compound. The yield is 50.0%. m.p.258-259°C; 1 H NMR (DMSO-d 6 , 300MHz) δ: 8.49(s, 1H, CH), 8.02(s, 1H, CH), 7.85~7.77(m, 4H, ArH), 7.29(d, J=5.0Hz, 2H, ArH), 7.23( d, J=2.7Hz, 1H, CH), 7.02(d, J=5.2Hz, 2H, ArH), 6.81(d, J=2.7Hz, 1H, CH), 4.75(t, J=4.7Hz, 2H ,-CH 2 ), 4.39 (t, J=5.0Hz, 2H, -CH 2 ), 2.48(s, 3H, CH 3 ).
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