40 results about "4-Chloroaniline" patented technology

The invention provides preparation of a semi-antigen and an artificial antigen and an antibody against herbicide anilofos, which relates to the semi-antigen, the artificial antigen and the antibody which have a basic structure of the herbicide anilofos. According to the invention, the antibody with good specificity to the herbicide anilofos is prepared by using an easy and convenient method. The antibody is prepared through the following steps: synthesizing the semi-antigen from N-chloracetyl-N-isopropyl-4-chloroaniline and mercaptoacetic acid; respectively connecting the semi-antigen with bovine serum albumin (BSA) and horseradish peroxidase (HRP) to synthesize the artificial antigen and an enzyme-labeled antigen; and subjecting the artificial antigen to animal immunization, blood drawing, separation of antiserum and purification so as to prepare the antibody. The antibody is stable and has good specificity and sensitivity; the synthetic method for the antibody is simple; and the antibody can be used for rapid immunodetection of residual herbicide anilofos in the environment, agricultural products and foodstuffs and has a good application prospect.

A provided preparation method for 4-chlorophenylhydrazine hydrochloride comprises the following steps: 1) under an acidic condition, at 5-10 DEG C, dropwise adding a sodium nitrite aqueous solution with a concentration of 20% into 4-chloroaniline to perform a diazo reaction and to generate a diazo salt; 2) under a room temperature condition, dropwise adding an ammonium sulfite aqueous solution into a solution of the diazo salt obtained in the step 1, heating to 50-60 DEG C and keeping the temperature for 3-4 h; and 3) at 50-70 DEG C, dropwise adding a hydrochloric acid solution with a concentration of 20% into the solution obtained in the step 2, keeping the temperature for 1-2 h, reducing the temperature, filtering, washing, discharging the material, and drying to obtain a finished product. The beneficial effects comprise that by using ammonium sulfite aqueous solution as a reducing agent in the reduction reaction, the problems are solved that sodium sulfite solid is easy to cake during material charging in a conventional technology and material charging is not easy to operate; ammonium chloride and ammonium hydrogen sulfate which are generated in the acidification reaction have high solubility in water, and crystallization precipitation is late, thereby facilitating performing of the acidification reaction in the solution and reducing side reactions; and the product crystallizes loosely, is good in fluidity, easy for material discharging and washing, and product quality and yield are both better than conventional production levels.

The invention provides a Pd complex catalyst as well as a preparation method and application thereof. The Pd metal complex catalyst provided by the invention has the structure shown by a formula (I), wherein R1 and R2 are alkyls or halogens; preferably, R1 is alkyl with 1-15 carbons, and R2 is alkyl with 1-5 carbons, or halogen; more preferably, R1 is methyl, ethyl, propyl or benzhydryl, and R2 is methyl or chlorine. DBCPh-NH2 is 2,6-bi (diphenylmethyl)-4-chloroaniline. According to the Pd metal complex catalyst, Heck reaction can be promoted when less Pd metal complex catalyst is used; and furthermore, the Pd metal complex catalyst has good catalytic performance and can be used for realizing the catalysis for the Heck reaction.

The invention relates to a method for preparing 2,5-dimethoxy-4-chloroaniline by using a liquid-phase catalytic hydrogenation method, which comprises the following steps: (a) under the solvent condition, performing a catalytic hydrogenation reaction by taking raneys nickel as a catalyst, dimethyl sulfoxide as an auxiliary agent, organic amine as a dehalogenation inhibitor and 2,5-dimethoxy-4-chloroaniline as a raw material in a high pressure reaction vessel; (b) carrying out decolorizing by using active carbon and filtering to a reaction solution obtained in a step (a), and then adding a protective agent into the reaction solution, cooling, crystallizing and filtering; (c) adding the protective agent into mother liquor filtered in a step (b), concentrating, cooling, crystallizing and filtering, then merging the obtained products filtered in the step (b) and step (c) to obtain the white 2,5-dimethoxy-4-chloroaniline. The invention has the advantages of clean reaction, less pollution, simple process, easy operation, less reaction energy consumption and low cost.

The invention discloses application of a 3-aryl-6-aryl-7H-thiazolo [3,2-b]-1,2,4-triazine-7-ketone derivative with a general formula I shown in the description to an antibacterial drug. In the general formula I, R1 and R2 are methyl, halogen, hydroxyl, methoxyl, acetyl, propionyl, formylphenyl, carbamoyl-methoxy-benzyl, 4-methylanilino formyl-methoxyl or chloroaniline formyl-methoxyl respectively and independently. The 3-aryl-6-aryl-7H-thiazolo [3,2-b]-1,2,4-triazine-7-ketone derivative, namely an antibacterial compound provided by the invention, has obvious inhibiting effects on methicillin-resistant staphylococcus aureus, escherichia coli, pseudomonas aeruginosa and a variety of bacteria, and can be used for the preparation of the antibacterial drug.

The invention provides a method for preparing 2,5-dimethoxy-4-chloroaniline by hydrogenation reduction, which comprises the following steps: (1) beating and dissolving a raw material of 2,5-dimethoxy-4-chloro nitrobenzene; (2) adding a catalyst and the material into a hydrogenation reactor, performing a relatively high temperature high pressure hydrogenation reaction in the early stage of the reaction; (3) transferring the material in the reaction of step (2) into a relatively low temperature low pressure reaction state; (4) after the reaction is complete, filtering the catalyst; (5) cooling and precipitating the material; (6) performing pressure filtration and precipitating the material to obtain the product. In the invention, the reduction process of 2,5-dimethoxy-4-chloroaniline is controlled to have two stages of a high temperature high pressure stage and a low temperature low pressure stage, which effectively controlled the dechlorination reaction, and realizes the selective reduction of nitro groups. Hydrogen reduction is adopted instead of iron powder reduction, which avoids the generation of a lot of iron mud, and reduces environment pollution.

The invention provides a synthetic method of hexamethylene flusulfamide. The synthetic method comprises the following steps: reacting to obtain 2-oxocyclohexyl ammonium sulphonate and ammonium sulfate by adopting cyclohexanone, 1, 4-dioxane, sulfur trioxide and ammonia as the raw materials; washing via reaction product through absolute methanol, and leaching to separate ammonium sulfate; and then carrying out reaction among 2-oxocyclohexyl ammonium sulphonate, oxalyl chloride and 2-trifluoromethyl-4-chloroaniline to obtain hexamethylene flusulfamide. According to the synthetic method provided by the invention, KOH solution is replaced via the ammonia, thus, the reaction endpoint is easily controlled; the byproduct ammonium sulfate can be used as chemical fertilizer after being separated, and the generation of three wastes such as waste barium sulfate can be removed; the reaction is easy to operate, the post-processing is simple to carry out, the product is high in purity and high in yield, and the method is suitable for large-scale industrial application.

The invention belongs to the organic synthesis field, and specifically relates to a synthetic method of 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one. According to the invention, the technical problems to be solved are low yield, high cost and difficult after-treatment purification of the existing synthetic method; a technical scheme for solving the technical problems is to provide a synthetic method of 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one; the synthetic method comprises the following steps of: carrying out an acylation reaction between 4-chloroaniline and succinic anhydride to obtain 4-(4-chloroaniline)-4-oxobutyric acid; carrying out an intramolecular Friedel-Craft reaction on 4-(4-chloroaniline)-4-oxobutyric acid to obtain 7-chloro-3,4-tetrahydrobenzo[b]azepine-2,5-one; reacting 7-chloro-3,4-tetrahydrobenzo[b]azepine-2,5-one with ethylene glycol to obtain 7-chloro-3,4-tetrahydrobenzo[b]azepine-2-one-5-glycol ketal; reducing 7-chloro-3,4-tetrahydrobenzo[b]azepine-2-one-5-glycol ketal, and carrying out de-ketalation under an acidic condition to obtain 7-chloro-1,2,3,4-tetrahydrobenzo[b]azepine-5-one. The invention provides a new method which is short in steps and high in total yield.

The invention relates to a preparation method of regorafenib. The method comprises the following steps: heating and melting 3-fluoro-4-nitrophenol and reacting with 4-chloro-N-methylpyridine-2-formamide under the action of KOH; reducing through hydrazine hydrate to obtain an intermediate I; finally enabling the intermediate I and 3-trifluoromethyl-4-chloroaniline, and ethylene carbonate to be subjected to one-pot reaction under the catalysis of a catalyst; carrying out post-treatment to obtain a regorafenib pure product. The method provided by the invention has the advantages of high conversion rate, safety and no harms, no pollution, moderate reaction conditions, high yield and high product purity, and is applicable to industrial production.

The invention relates to a method for synthesizing 2,5-dimethoxy-4-chloroaniline. The method comprises the steps: in the presence of carbon oxide and water, performing the reaction in an organic solvent under a high temperature and high pressure by adopting 2,5-dimethoxy-4-chloro-nitrobenzene as a raw material, selenium as a catalyst and organic alkali or inorganic alkali as an assistant catalyst, and reducing the nitro to amino to synthesize the 2,5-dimethoxy-4-chloroaniline. The method adopts high-pressure reaction and one-pot reaction, so that less equipment investment is needed, the operation is simple and convenient, and a product is relatively easy to separate and purify.

The invention discloses an imidazo[1,2-a]pyridine near-infrared ratio type pH fluorescence probe, a preparation method of the probe and application of the probe in measuring the extremely-acid pH change in living cells and escherichia coli. Under inert gas protection, 4-dimethylamino-cinnamaldehyde or a derivative thereof, 4-chloroaniline and sodium bicarbonate are dissolved in methyl alcohol, andafter a heating reflux reaction is conducted, a reaction product and 2-(4-methoxyphenyl)-7-methyl imidazo[1,2-a]pyridine are dissolved in N,N-dimethylformamide; potassium tert-butoxide is taken as analkaline reagent, and a heating reflux reaction is conducted; after concentration, silicagel column separation is conducted. Under the extremely acid condition, a transmitted wave of the probe is longer than 600 nanometers, the transmitted wave is located in a near infrared region, a ratio transmission fluorescence characteristic is presented, and the probe has the advantages of high sensitivityand good selectivity for H+, large Stokes displacement and the like.

The invention discloses a preparation method of 4-Chloro-2,5-dimethoxyacetoace tanilide. The preparation method particularly comprises the following steps: adding an alcohols solvent or an acetic acid solvent into a reactor, meanwhile, adding 2,5-dimethoxy-4-chloroaniline, controlling the temperature to be 10-100 DEG C, dripping acetyl ketene, and finishing adding after 0.5-4 h, wherein the molar ratio of 2,5-dimethoxy-4-chloroaniline to acetyl ketene is 1:1-1:1.2; and after finish of dripping, preserving the temperature for 0.5-4 h, keeping the material in a fully-dissolved state after finish of reaction, adjusting the pH to be 0.5-5.0, quickly cooling with a refrigerating fluid, quickly stirring, controlling the cooling speed to be 5-40 DEG C/min, enabling 4-Chloro-2,5-dimethoxyacetoace tanilide to be quickly separated out as powder, cooling to -10 DEG C to 20 DEG C, filtering and drying obtain 4-Chloro-2,5-dimethoxyacetoace tanilide. The preparation method is simple, and the enolic isomer content in obtained 4-Chloro-2,5-dimethoxyacetoace tanilide can be controlled to be 50 ppm or below.

The invention relates to a preparation method of sorafenib. The method comprises the following steps of allowing p-nitrophenol and 4-chlorine-N-picoline-2-formamide to react under the action of anhydrous potassium carbonate and PEG (polyethylene glycol)-400, generating a compound I via hydrazine hydrate reduction, allowing the compound I, 3-trifluoromethyl-4-chloroaniline and diphenyl carbonate orN,N-disuccinimidyl carbonate to give a 'one-pot' reaction by the action of a catalyst, performing post-treatment to form a sorafenib crude product, and performing further purification to form pure sorafenib. The method is high in conversion rate, safe, free from harm and pollution, mild in reaction condition, high in yield and applicable to industrial production, and can ensure high product purity.

The invention provides a synthesis method of chesulfamide. The method includes the steps of: reacting the halogenation product 2-halogenated cyclohexanone of cyclohexanone with sulfite to obtain 2-cyclohexylsulfonate; then carrying out reaction with oxalyl chloride, 2-trifluoromethyl-4-chloroaniline to obtain chesulfamide. In the invention, 2-halogenated cyclohexanone and sulfite are employed to substitute cyclohexanone and sulfur trioxide.1, 4-dioxane compound, thus avoiding the problems that the end point of chemical reaction for removal of SO4<2-> with precipitant BaCl2 or Ba(OH)2 is hardlycontrollable and the generated BaSO4 precipitate cannot be utilized and become three wastes, and overcoming the disadvantages of corrosion, difficult storage, difficult operation, strong irritating odor, easy cause of poisoning and the like of ammonia gas. The method provided by the invention has the advantages of mild reaction conditions, simple operation, high product purity and high yield, andis suitable for large-scale industrial application.

The invention relates to an efficient synthesis method of 5-chlorobenzotriazole. The method comprises the following steps of (1) adding 2-nitro-4-chloroaniline, water and catalysts of raney nickel into a reaction kettle for reaction; performing climbing plate detection to obtain completely reacted materials; (2) performing filtering and reduced pressure dewatering on the completely reacted materials to obtain 4-chloro-1,2-diaminobenzene materials and waste water A; (3) adding the 4-chloro-1,2-diaminobenzene materials and sodium nitrite into a medium pressure reaction kettle; adding water; performing heat release reaction to obtain a 5-chlorobenzotriazole sodium salt water solution; (5) dripping sulphuric acid into the 5-chlorobenzotriazole sodium salt water solution; performing filtering and spin drying to obtain a 5-chlorobenzotriazole coarse product and waste water B; (5) washing and drying the 5-chlorobenzotriazole coarse product to obtain washing water and a finished product of 5-chlorobenzotriazole with the content being higher than or equal to 99 percent; (6) mixing the waste water A, the waste water B and washing water; then, performing negative pressure distillation to obtain distilled water and waste slag; returning the distilled water into the step (1); dewatering the waste slag to obtain a byproduct of sodium sulfate with the content being higher than or equal to 96percent. The method has the advantages of low cost, low energy consumption and high earnings.

The invention discloses a medical aluminum foil packaging film. The medical aluminum foil packaging film comprises a printing layer, an outer film layer, a first adhesive layer, an aluminum foil layer, a second adhesive layer and a heat sealing layer which are arranged in sequence from outside to inside. The first adhesive layer and the second adhesive layer are both prepared from, by weight, 5-10 parts of acetic ether, 2-5 parts of a formaldehyde solution, 2-4 parts of polypropylene fibers, 2-6 parts of butyraldehyde anilin-econdersate, 1-3 parts of a vulcanizing agent, 2-5 parts of nano-silica, 30-45 parts of polyurethane resin, 1-3 parts of spice, 2-6 parts of nano-scale europium oxide, 2-6 parts of 2-amino-4-chloroaniline, 1-3 parts of boric acid, 2-5 parts of dodecyl diacyl polyethylenimine and 5-10 parts of water. In this way, the adhesive layers of the medical aluminum foil packaging film are good in flexibility, and the overall usability is improved.