Novel microtube reaction technology for synthesizing metronidazole bulk drug, and application thereof
A technology of microtubule reaction and metronidazole, which is applied in the direction of organic chemistry, can solve the problems of lower product yield, poor gas-liquid two-phase mixing effect, product dehydration, etc., to improve product selectivity, reduce the amount of acid, The effect of increasing the yield
Pending Publication Date: 2020-01-10
HUBEI UNIV
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[0004] However, there are many shortcomings in the tank reaction: (1) the gas-liquid two-phase mixing effect of the tank reactor is poor, and ethylene oxide is easy to escape from the system; (2) the amount of sulfuric acid is large, and a large amount of ethylene oxide is consumed, resulting in A large amount of ethylene glycol and its polymers also lead to an increase in the amount of alkali used for neutralization, resulting in a large amount of waste salt wastewater; (3) The strong acidic reaction condition takes a long time to react, resulting in dehydration, esterification or etherification of some products, which reduces the product quality. yield
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[0032] (1) Under 90-95 DEG C of water bath conditions, slowly add 100 grams of 2-methyl-5-nitroimidazole to the mixed acid of 100 grams of 85% formic acid and 50 grams of 98% concentrated sulfuric acid (mass ratio 2: 1), stir until all the solids are dissolved, and prepare a 40% nitro substance raw material solution for use.
[0033] (2) The coil with an inner diameter of 4mm is placed in a medium at 95°C, either in an oil bath or in a water bath. Two metering pumps are used to respectively feed the nitro raw material hot solution and ethylene oxide cryogenic liquid into the mixing section of the coil reactor under the condition of heat preservation, and the pressure of the metering pump is used to push the liquid to flow. The feed rate of ethylene oxide was controlled by a metering pump to 4 ml / min and the molar ratio of feeding was 2-methyl-5-nitroimidazole: ethylene oxide=1:2. The reaction mixture was collected at 15 meters from the coil, and the reaction time was about 15...
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The invention belongs to the technical field of medicine manufacturing, and particularly relates to a novel microtube reaction technology for synthesizing a metronidazole bulk drug, and an applicationthereof. The novel production technology is provided to overcome the defects of existing industrial production technologies of metronidazole. The technology mainly comprises the following steps: preparing a high-concentration mixed acid solution of 2-methyl-5-nitroimidazole under a high-temperature condition, wherein the mixed acid is a mixed solution of formic acid and concentrated sulfuric acid; respectively and simultaneously feeding the mixed acid solution and ethylene oxide into a miniature coil pipe, performing a reaction, and placing the miniature coil pipe in a 90-95 DEG C liquid medium; carrying out reduced pressure distillation to obtain a reaction concentrate; diluting the reaction concentrate, neutralizing the reaction concentrate until the pH value is 2.0-2.5, and cooling andfiltering the neutralized concentrate; neutralizing the obtained filtrate until the pH value is 10-11, cooling and filtering the neutralized filtrate, and washing the obtained filter cake with wateruntil the filter cake is neutral to obtain a crude product; and recrystallizing and decolorizing the crude product to obtain refined metronidazole. The technology has the advantages of mild process conditions, short reaction time, high safety, and suitableness for continuous industrial production.
Description
technical field [0001] The invention belongs to the technical field of medicine manufacturing, and in particular relates to a novel microtubule reaction process for synthesizing metronidazole bulk drug and its application. Background technique [0002] Metronidazole (Metronidazole, molecular formula: C 6 h 9 N 3 o 3 , CAS No.: 443-48-1), Chinese name: 1-(2-hydroxyethyl)-2-methyl-5-nitroimidazole, commonly known as metronidazole, nitroxyzol, or mitidine azoles, etc., are mainly used to treat or prevent systemic or local infections caused by anaerobic bacteria, such as anaerobic bacterial infections in the abdominal cavity, digestive tract, female reproductive system, lower respiratory tract, skin and soft tissues, bones and joints, etc. Endocarditis, meningeal infection, and colitis caused by antibiotics are also effective. The treatment of tetanus is often combined with tetanus antitoxin, and it can also be used for oral anaerobic infections. [0003] At present, the i...
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IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 胡泉源张震宇武成城赵涛涛
Owner HUBEI UNIV