- Preparation method of imidocarb dipropionate and intermediate thereof
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The invention discloses a preparation method of imidocarb dipropionate and an intermediate thereof and belongs to the technical field of chemical pharmacy. According to the method, m-nitrobenzonitrilereacts with ethylenediamine with sodium sulfide taken as a catalyst; palladium on carbon-ammonium formate reduction is performed; a product and urea are subjected to condensation reaction, so that imidazole phenylurea dihydrochloride can be obtained; dissociated imidazole phenylurea reacts with propionic acid, so that the imidazole phenylurea dipropionate can be obtained. The method has the advantages o reduced wastes, cheap and easily available raw materials, simple operation, high product yield, simple process operation and high safety, and is suitable for industrial production.
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- Preparation method of 2-(3-amino phenyl) imidazoline hydrochloride and imidocarb
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The invention relates to the field of chemical engineering and discloses a preparation method of 2-(3-amino phenyl) imidazoline hydrochloride and imidocarb. The preparation method comprises the following steps of: inputting 2-(3-nitryl phenyl) imidazoline, a catalyst and an alcohol-water mixed solution into a reaction kettle, stirring the mixture and raising the temperature to 50-65 DEG C, keeping the temperature and stirring the mixture for 10-20 min to obtain a mixed solution M; dropwise adding formic acid into the solution M, and keeping the temperature to react for 1.5-2.5h to obtain a mixed solution N; cooling the solution N to 40 DEG C below and filtering the solution, and evaporating alcohol to obtain a 2-(3-amino phenyl) imidazoline aqueous solution; dropwise adding hydrochloric acid into the 2-(3-amino phenyl) imidazoline aqueous solution to be neutral; and performing crystallization, suction filtration, pressure reduction and drying to obtain a target product 2-(3-amino phenyl) imidazoline hydrochloride. Compared with catalytic hydrogenation in the prior art, by taking formic acid as a hydrogen donor for transfer hydrogenation, the product purity and yield are of no obvious differences but no safety risks are available, and the preparation method is free of special demand, easy to operate and convenient for production and application.
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- A process for the preparation of imidazole
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The invention relates to a preparation method of imidocarb. The preparation method comprises the steps of dissolving methyl-m-nitrobenzoate into a solvent, enabling methyl-m-nitrobenzoate and ethylenediamine to be subjected to cyclization reaction at the temperature of 55-65 DEG C for 3-6h under the action of a catalyst, and separating to prepare m-nitroimidazoline; dissolving m-nitroimidazoline into a water solution of methanol, adding zinc powder under an acidic condition, after the addition is ended, carrying out reduction reaction for 1-2h while stirring at normal temperature, and separating and purifying to prepare m-aminoimidazoline; dissolving m-aminoimidazoline into a water solution of tetrahydrofuran, regulating the pH value to 7-10, adding triphosgene, reacting at the temperature of 10-40 DEG C for 2-6h, filtering and drying to obtain imidocarb. Methyl-m-nitrobenzoate is used as a starting raw material, and zinc powder is used as a reducing agent, so that the preparation method is mild in reaction condition, convenient in operation and relatively low in cost.
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Paragraph 0030; 0032
(2016/10/07)
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