12 results about "Nitrochlor" patented technology

The present application relates to the technical fields of medicine and intermediate preparation, and particularly relates to a synthesis method of 2-cyclopropylamino-3-nitro-6-chloropyridine. The preparation method comprises the following steps: taking 2,6-dichloro-3-nitropyridine and cyclopropylamine as raw materials, taking silica gel as a catalyst, and performing substitution reaction on 2,6-dichloro-3-nitropyridine and cyclopropylamine in the presence of the catalyst and an organic solvent to obtain 2-cyclopropylamino-3-nitro-6-chloropyridine. In view of the problems of poor reaction selectivity, cumbersome purification operation and difficulty in amplification existing in the preparation of 2-cyclopropylamino-3-nitro-6-chloropyridine, the present application uses silica gel as a catalyst, greatly reduces the generation of by-products, improves the reaction selectivity and yield, avoids the use of column chromatography purification, and only needs to be beaten to obtain qualified products.

The invention provides a method for preparing p-aminobenzoic acid through chlorination, hydrolysis and hydrogenation of p-nitrotoluene, and belongs to the technical field of organic compound preparation. Comprising the following steps: melting p-nitrotoluene, and performing chlorination reaction under the catalysis of azodiisobutyronitrile to generate a chlorinated product containing p-nitrobenzyl chloride; mixing the chlorination product with liquid caustic soda and sodium hypochlorite for hydrolysis reaction, separating liquid after reaction, and acidifying an upper-layer water phase to obtain p-nitrobenzoic acid; the method comprises the following steps: mixing p-nitrobenzoic acid with methanol and a Pd / C catalyst, carrying out hydrogenation reaction in a hydrogen environment, and filtering, distilling, cooling, centrifuging and drying after the reaction to obtain p-aminobenzoic acid. The method is simple in process route, mild in reaction condition, high in product purity, high in yield and suitable for industrial production, raw materials are easy to obtain, hydrogen chloride gas generated in the chlorination reaction and p-nitrotoluene obtained after the hydrolysis reaction are recycled, cyclic utilization of resources is achieved, and the production cost is reduced.

The invention relates to the technical field of synthesis of organic compounds, and particularly discloses a synthesis process of paranitroaniline. The synthesis process comprises the following steps: (1) preparing strong ammonia water with the concentration of 38-42% by using an ammonia water preparation unit; (2) adding p-nitrochlorobenzene, stronger ammonia water and an auxiliary agent into the reaction kettle, and then carrying out heat preservation reaction for 14-16 hours under the conditions that the temperature is 150-170 DEG C and the pressure is 5.6-6.2 MPa; the auxiliary agent comprises modified cyclodextrin and trehalose; and (3) transferring the material in the reaction kettle into a water washing kettle after pressure relief, carrying out water washing stirring for 1-2 hours, and carrying out centrifugal separation on the material liquid after water washing to obtain p-nitroaniline. According to the synthesis process disclosed by the invention, the problem of balance between main reaction efficiency and side reaction inhibition is solved from a reaction mechanism level through compounding and synergy of the modified cyclodextrin and the trehalose, and finally, high yield and high purity in the paranitroaniline synthesis process are synchronously achieved.

The application relates to the technical field of organic compound synthesis, and particularly discloses a synthesis process of p-nitroaniline. The synthesis process of p-nitroaniline comprises the following steps: (1) preparing concentrated ammonia water with a concentration of 38%-42% by using an ammonia water preparation unit; (2) adding p-nitrochlorobenzene, concentrated ammonia water and an additive into a reaction kettle, and then carrying out heat preservation reaction under the condition of 150-170 DEG C and 5.6-6.2 MPa for 14-16 h; the additive comprises modified cyclodextrin and trehalose; (3) after pressure relief, the materials in the reaction kettle are transferred into a water washing kettle to carry out water washing and stirring for 1-2 h, and the material liquid after water washing is subjected to centrifugal separation to obtain p-nitroaniline. According to the synthesis process, the modified cyclodextrin and the trehalose are compounded and synergized, the balance problem of the main reaction efficiency and the side reaction inhibition is solved from the reaction mechanism level, and finally the high yield and the high purity in the synthesis process of p-nitroaniline are simultaneously achieved.

The embodiment of the invention relates to a method for synthesizing 2-nitro-6-chlorotoluene, and belongs to the technical field of organic synthesis. According to the method, 2-nitrotoluene and chlorine are used as raw materials, a tubular reactor or a common reactor is used as reaction equipment, chlorination is carried out at 10-50 DEG C under the condition of 180-400 nm ultraviolet irradiation, a mixture of 2-nitro-4-chlorotoluene and 2-nitro-6-chlorotoluene is obtained, rectification separation and purification are carried out, and 2-nitro-6-chlorotoluene is obtained. The method has the advantages of cheap and easily available raw materials, simple reaction operation, simple post-treatment, greenness, environmental protection, small pollution generated in the production process, realization of continuous production, reuse of unreacted raw materials, and substantial reduction of the cost.

The invention relates to a synthesis method of 2-nitro-4-methylsulfonyl toluene, which comprises the following steps: reacting 2-nitro-4-chlorotoluene with sodium methyl mercaptide and other raw materials to synthesize 2-nitro-4-methylthio toluene, and oxidizing to obtain 2-nitro-4-methylsulfonyl toluene, the synthesis route is simple, the problem of large amount of waste acid and waste water is solved, and the synthesis method is green and environment-friendly.

The invention relates to a novel method for synthesizing 3-chloro-2-methylaniline, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking 2-nitro-6-chlorotoluene and hydrogen as raw materials and taking a tubular reactor or a common reactor as reaction equipment, carrying out hydrogenation reaction at 60-150 DEG C to obtain a 3-chloro-2-methylaniline crude product, and carrying out melt crystallization and purification to obtain the 3-chloro-2-methylaniline. The method has the advantages of cheap and easily available raw materials, simple reaction operation, simple post-treatment, greenness, environmental protection, small pollution generated in the production process, realization of continuous production, reuse of unreacted raw materials, and substantial reduction of the cost.

The invention provides a method for separating p-nitrochlorobenzene from o-nitrochlorobenzene and m-nitrochlorobenzene in a chlorobenzene nitration product. The separation method comprises the following steps: step 1, introducing a chlorobenzene nitration product into a moving bed filled with an adsorbent, and selectively adsorbing m-nitrochlorobenzene to obtain a raffinate phase without meta-isomers and an adsorption phase rich in m-nitrochlorobenzene; step 2, desorbing the adsorption phase by using a desorption agent to obtain a desorption solution, carrying out reduced pressure rectification on the desorption solution, collecting an m-nitrochlorobenzene product at a tower kettle, and obtaining a regenerated desorption agent at the tower top for recycling; step 3, carrying out melt crystallization on the raffinate phase, and separating to obtain a p-nitrochlorobenzene product and crystallization mother liquor; and step 4, rectifying the crystallization mother liquor to obtain an o-nitrochlorobenzene product at a tower kettle. By adopting the separation method disclosed by the invention, the purity of para-nitrochlorobenzene, ortho-nitrochlorobenzene and meta-nitrochlorobenzene is greater than 99.2%, the purity of meta-nitrochlorobenzene is not less than 75%, the energy consumption is remarkably reduced, and the benefit is improved.

The invention relates to an industrial preparation method for synthesizing 2-nitro-5-chloropyridine under the catalysis of a copper salt / ligand. Specifically, the invention discloses a preparation method for preparing 2-nitro-5-chloropyridine by carrying out an intermolecular C-N bond coupling reaction on 2, 5-dichloropyridine or 2-bromo-5-chloropyridine and nitrite under the action of a catalyst and alkali in an inert solvent, and the method has the advantages of simple operation, easily available raw materials, environmental friendliness, high catalytic efficiency, high yield, high purity, high yield and the like. The method has the characteristics of high reaction yield, good product purity and the like, and is easy for industrial production.

The invention discloses a preparation method of high-purity clofazimine, and belongs to the technical field of drug synthesis, the key points of the technical scheme are as follows: S1, parachloroaniline, 2-fluoronitrobenzene and triethylamine are mixed and then react at 120-130 DEG C for 4.5-5.5 h, cooling is performed, absolute ethyl alcohol is added, and cooling is performed to room temperature to obtain 2-nitro-4 '-chlorodiphenylamine; s2, reducing nitryl of the 2-nitro-4 '-chlorodiphenylamine into amino, so as to obtain 2-amino-4'-chlorodiphenylamine; s3, reacting the 2-amino-4 '-chlorodiphenylamine under the action of ferric trichloride, absolute ethyl alcohol and hydrochloric acid for 9-10 hours to obtain iminophenazine hydrochloride; s4, carrying out an addition-elimination reaction on the 2-parachloroanilino-5-parachlorophenyl-3, 5-dihydro-3-iminophenazine hydrochloride, so as to obtain a clofazimine crude product; s5, refining the clofazimine crude product to obtain the high-purity clofazimine, the purity of the clofazimine reaches 99% or above by adjusting reaction parameters in each step, the clofazimine can be basically dissolved in gastric juice 60 minutes later, and the absorption efficiency is improved.

This invention belongs to the field of pharmaceutical synthesis technology, specifically relating to a method for preparing chloroprocaine hydrochloride and its intermediates, and their applications. The invention uses 2-chloro-4-nitrobenzoic acid and N,N-diethylethanolamine as starting materials, and prepares nitrochlorocaine via sulfuric acid-catalyzed esterification. Nitrochlorocaine is then reduced with thiourea dioxide to obtain crude chloroprocaine. The crude chloroprocaine is then salted in hydrochloric acid and ethanol, crystallized, and dried to obtain the final product, chloroprocaine hydrochloride. This method features low cost, high product quality, high yield, simple process, high production capacity, environmental friendliness, and suitability for industrial production, thus possessing significant industrialization value.

This invention provides a catalyst for catalyzing the cycloaddition reaction of carbon dioxide and a method for its preparation. The catalyst has the structural formula: [formula omitted for brevity], where poly[formula omitted for brevity]. core For polystyrene core, poly shell For the polychloromethylstyrene shell, Cation N + indicates a nitrogen-containing cationic group; Anion O - represents a phenolic oxide anionic group; wherein the structural formula of the phenolic oxide anionic group is: , where R3 is any one of hydrogen, hydroxyl, methoxy, amino, nitro, and chlorine. This catalyst is easy to recover, has good stability, and exhibits good catalytic effect.