Method for synthesizing secnidazole and secnidazole
A technology for synthesizing secnidazole and secnidazole, which is applied in organic chemistry and other fields, can solve problems such as high reaction temperature and acid waste gas corrosion, and achieve the effects of short reaction time, reduced corrosion, and reduced energy consumption
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Embodiment 1
[0030] This embodiment provides a method for synthesizing secnidazole, comprising the following steps:
[0031] Add 2-methyl-5-nitroimidazole, 1-bromo-2-propanol, potassium carbonate, and acetone at a molar ratio of 1:2:2.1:14 into a 10L glass reactor, in which 2-methyl- The mass of 5-nitroimidazole is 635g, the mass of 1-bromo-2-propanol is 1380g, the mass of potassium carbonate is 1480g, and the volume of acetone is 5L.
[0032] Under the condition of stirring, the reaction was refluxed for 4 hours, and the reaction temperature was 60°C; according to the TLC detection (developing condition: GF254 silica gel plate, developing agent chloroform: ethanol = 85:15) the reaction termination point, the reaction mixture A was obtained.
[0033] Recover the acetone in the reaction mixture A to obtain the reaction mixture B; add 6L of water to the reaction mixture B, cool the reaction mixture B to 3°C, and centrifuge to obtain a wet product; stir and wash the wet product with water at a ...
Embodiment 2
[0037] This embodiment provides a method for synthesizing secnidazole, comprising the following steps:
[0038] Add 2-methyl-5-nitroimidazole, 1-bromo-2-propanol, potassium carbonate, and acetone at a molar ratio of 1:3:3:20 into a 10L glass reactor, in which 2-methyl- The mass of 5-nitroimidazole is 635g, the mass of 1-bromo-2-propanol is 2070g, the mass of potassium carbonate is 2114g, and the volume of acetone is 7.1L.
[0039] Under the condition of stirring, reflux reaction for 5 hours, the reaction temperature is 70°C; according to the TLC detection (development condition: GF254 silica gel plate, developer chloroform: ethanol = 85:15) the reaction termination point, the reaction mixture A was obtained.
[0040] Recover the acetone in the reaction mixture A to obtain the reaction mixture B; add 9L of water to the reaction mixture B, cool the reaction mixture B to 0°C, and centrifuge to obtain a wet product; stir and wash the wet product with water at a temperature of 1°C ...
Embodiment 3
[0044] This embodiment provides a method for synthesizing secnidazole, comprising the following steps:
[0045] Add 2-methyl-5-nitroimidazole, 1-bromo-2-propanol, potassium carbonate, and acetone at a molar ratio of 1:1.5:2:7 into a 10L glass reactor, in which 2-methyl- The mass of 5-nitroimidazole is 635g, the mass of 1-bromo-2-propanol is 1035g, the mass of potassium carbonate is 1410g, and the volume of acetone is 2.5L.
[0046] Under the condition of stirring, reflux reaction for 3 hours, the reaction temperature is 70°C; according to the TLC detection (development condition: GF254 silica gel plate, developer chloroform: ethanol = 85:15) the reaction termination point, the reaction mixture A was obtained.
[0047] Recover the acetone in the reaction mixture A to obtain the reaction mixture B; add 3L of water to the reaction mixture B, and cool the reaction mixture B to 2°C, centrifuge to obtain a wet product; stir and wash the wet product with water at a temperature of 2°C...
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