101 results about "P-chlorobenzaldehyde" patented technology

The invention discloses a phosphorus-nitrogen swelling type fire retardant and a method for preparing the same. The chemical name of the fire retardant is 5, 5-dimethyl-4-p-chlorophenyl-1, 3, 2-dioxaphosphorinane phosphonate melamine salt. The preparation method comprises the following steps: (1) p-chlorobenzaldehyde and iso-butyraldehyde react with alkali ethanol solution, are cooled down and filtered to obtain an intermediate product (I); (2) the intermediate product (I) and phosphoric acid are added to solvent, and added with paratoluenesulfonic acid or benzoic acid or sodium salt of benzoic acid; and the mixing solution is distilled after reaction to reclaim the solvent to obtain an intermediate product(II); and (3) melamine and the intermediate product(II) are added to water for reaction, cooled down and filtered to obtain a filter cake; and the filter cake is dried to obtain phosphorus-nitrogen swelling type fire retardant. The phosphorus-nitrogen swelling type fire retardant has the advantages of high thermal stability, good compatibility, no halogen, less smoke and environmental protection. The preparation method has the advantages of materials available, simple process, mild reaction conditions, small viscosity of reaction liquid, low requirement on equipment and little environmental pollution.

The invention discloses a preparation method of p-methylsulfonyl benzaldehyde, which takes p-chlorobenzaldehyde as starting material, and comprises the steps of: enabling the starting material to have reaction with sodium methyl mercaptide water solution under the action of phase transfer catalyst to obtain p-methylthio benzaldehyde; and oxidizing the p-methylthio benzaldehyde by hydrogen peroxide under the action of sulfuric acid and oxidation catalyst to obtain the p-methylsulfonyl benzaldehyde. The preparation method is easy in obtaining of raw material of the p-methylsulfonyl benzaldehyde, simple and convenient in operation, low in cost, high in yield and suitable for industrial production.

The invention discloses a preparation method of tebuconazole. The preparation method using p-chlorobenzaldehyde and pinacolone as initial raw materials comprises the following steps of: obtaining 2-(4-chlorobenzene ethyl)-2-tertiary butyl ethylene oxide through condensation reaction, hydrogenation reaction and epoxidation reaction in sequence; obtaining tebuconazole through ring-opening reaction of 2-(4-chlorobenzene ethyl)-2-tertiary butyl ethylene oxide and triazole under the co-catalysis of organic amine and crown ether. A catalysis technology of a composite catalyst which is composed of organic amine and crown ether is adopted, so that the isomer byproducts in the ring-opening reaction are greatly reduced, the ring-opening yield is improved to 92.8% from 80% of the conventional process, the product quality is improved to 98.5% or higher from 95%, and the total yield (in terms of p-chlorobenzaldehyde) is improved to 82% or higher from 65% of the conventional process.

The present invention relates to a catalyst for preparation of p-chlorobenzaldehyde through liquid phase catalytic oxidation. The catalyst is a compound catalyst, which is formed by loading an element provided with catalytic activity on a carrier of aluminum oxide. Active componentS of the catalyst of the present invention are cobalt and manganese, which are loaded on the carrier of the aluminum oxide. The molar ratio of cobalt and manganese is 0.1-5. In addition, the active components of the present invention can also comprise nickel, copper, iron, cerium, lanthanum, magnesium or zirconium and bromine, besides cobalt and manganese. The catalyst of the present invention is applied the reaction course for preparation of p-chlorobenzaldehyde, and is characterized by the simple technique, the high p-chlorobenzaldehyde reaction yield ratio, the low reaction temperature, the simple catalyst separation, and so on.

The invention discloses high purity metconazole and a preparation method thereof; the preparation is as follows: exocyclic double bond alpha, beta-unsaturated ketone (II) can be obtained by condensation reaction of cyclopentanone and p-chlorobenzaldehyde; then the exocyclic double bond alpha, beta-unsaturated ketone (II) is reacted with a methylation reagent to obtain alpha', alpha'-dimethyl substituted exocyclic double bond alpha, beta unsaturated ketone (III); then in the presence of a catalyst, the alpha', alpha'-dimethyl substituted exocyclic double bond alpha, beta unsaturated ketone (III) is reacted with hydrogen to obtain 2, 2-dimethyl-5-(4-chloro-benzyl) cyclopentanone (IV) with the double bond being reduced; an epoxypropane compound (V) is obtained by Johnson-Corey-Chaykovsky of the reduced product (IV); finally the epoxypropane compound (V) is reacted with 1, 2, 4 - triazole, and then the high purity metconazole (I) can be obtained by recrystallization. The preparing method has the advantages of chip and easy available raw materials, short route, good selectivity, high overall yield and good atom economy, and is very suitable for industrial production.

The invention discloses a combined purification method of o/p-chlorobenzaldehyde rectification raffinate and process wastewater. The method concretely comprises the following steps: adding a dispersant to the rectification raffinate and process wastewater to reduce the viscosity in order to form a dispersion; allowing the dispersion to enter a fluidized bed reactor and undergo catalytic cracking oxidation, and allowing the obtained dispersiont o enter a fixed bed reactor and undergo catalytic oxidation purification; carrying out heat transfer condensation and gas-liquid separation on the obtained fixed bed outlet gas, allowing the obtained liquid to enter a neutralization tank, neutralizing HCl and Cl2 dissolved in the liquid by a diluted alkali solution, discharging neutralized liquid to a rain discharging system, allowing the gas to enter an alkali solution absorption tower to absorb HCl and Cl2 in the gas, and directly discharging the absorbed gas to air. The method allows the rectification raffinate and process wastewater to be simultaneously treated at a low temperature through a raffinate emulsification-fluidized bed catalytic cracking oxidation-fixed bed catalytic oxidation purification technology, the content of VOCs in the treated gas is less than 45 mg/m<3>, the content of CODs in the liquid does not exceed 80 mg O2/L, and the high-efficiency, low-cost and low-energy consumption treatment of the rectification raffinate and the process wastewater is realized in a one-step manner.

The invention relates to a novel method for preparing metconazole. The method takes p-chlorobenzaldehyde and 2-methoxycarbonyl cyclopentanone represented by the formula (1) as the primary raw materials, then after a series of reactions, obtains an intermediate of metconazole, namely 5-(4-chlorobenzyl)-2,2-dimethyl cyclopentanone represented by the formula (5); then subjects the intermediate to reacts with trimethylsulfonium bromide so as to obtain a reaction product, and finally subjects the reaction product to react with 1,2,4-1H-triazole so as to obtain the metconazole. The preparation method has the advantages of simple technology, available raw materials, low cost, little discharge of waste water, waste gas, and waste solid, and high content and yield of target product metconazole, wherein the metconazole content can reach 95% or more, and the total yield can reach 65% or more, and is suitable for industrial production.

The invention relates to a method for synthesizing a broad spectrum antibiotic of chloramphenicol. The method comprises the following steps of: synthesizing (R)-2-nitro-1-(4-chlorophenyl)ethanol by using p-chlorobenzaldehyde and nitromethane as raw materials in the presence of a chiral catalyst; reacting with formaldehyde to obtain (1R,2R)-2-nitro-1-(4-chlorophenyl)-1,3-propanediol, and performing catalytic hydrogenation to obtain (1R,2R)-2-amino-1-(4-chlorophenyl)-1,3-propanediol; and performing nitro substitution and dichloro acetylization on the intermediate to obtain the chloramphenicol. By the method, the common chiral resolution and aluminum isopropoxide reduction in the industry at present can be avoided, three wastes are reduced, the raw materials and reagents are cheap and readily available, the method comprises a few synthesizing steps, the yield is high, and the method is more suitable for industrial production.

The invention discloses a semisynthesis process for producing benflumetol by taking alpha (di-n-butylamide)-2,7-dichloro-4-fluorenemethanol as a raw material. The process comprises the following steps: dispersing alpha (di-n-butylamide)-2,7-dichloro-4-fluorenemethanol in a mixed solvent, carrying out alkali catalysis and heating reflux on the obtained mixture, and carrying out condensation reaction on the obtained object and p-chlorobenzaldehyde, reducing the temperature to room temperature, and continuing to stir the obtained product so as to separate out coarse benflumetol grains; carrying out recrystallization on the coarse benflumetol grains by using acetone crystallization so as to obtain a fine benflumetol product with a content and a purity of more than 99.0%.

The invention discloses a method for preparing p-chlorobenzaldehyde, which comprises the following steps: reacting p-chlorotoluene with chlorine in the presence of an initiator under the irradiation of a mercury lamp at the chlorination temperature of 90-140 DEG C to obtain a p-chlorobenzyl chloride/p-trichlorotoluene mixture; and while controlling the average chlorination degree at 1.4-1.6, carrying out catalytic hydrolysis in a 3-6 wt% nitric acid solution for 6-12 hours to obtain the p-chlorobenzaldehyde. By using the method disclosed by the invention, the next hydrolysis step can be directly carried out without separating the intermediate; and thus, the method is simple in technique and can easily implement industrialized production.

The invention provides 7-(4-chlorphenyl)-5,6-dihydro-7aH-benzo[h]1,2,4-triazolo[3,4-b]quinazoline-5,6-diketone and a synthetic method thereof. The method comprises the following steps of: uniformly mixing 3-amino-1,2,4-triazole, p-chlorobenzaldehyde, 2-hydroxyl-1,4-naphthaquinone and p-methylbenzene sulfonic acid with a usage amount of catalyst, heating and stirring, controlling the temperature at 110-125 DEG C and reacting for 2.5-3 hours. The 7-(4-chlorphenyl)5,6-dihydro-7aH-benzo[h]1,2,4-triazolo[3,4-b]quinazoline-5,6-diketone prepared according to the invention introduces chlorine atoms, thus having stronger activity and being more beneficial to absorption. The method provided by the invention is green and environment-friendly, and has the characteristics that the raw materials are available, the operation is simple and the yield is high.

The invention provides a preparation method of p-chlorophenylglycine, which comprises the following steps: adding a mixed solution of a chloroform solution, a catalyst and p-chlorobenzaldehyde into asodium hydroxide solution, mixing, and dropwisely adding liquid ammonia while stirring for 2-6 hours; after finishing dropwise adding the liquid ammonia, adding an ammonium bicarbonate solution, and reacting for 5-10 hours at room temperature; after the reaction is finished, distilling and concentrating a reaction solution, decolorizing and filtering by using activated carbon, adjusting the pH value of a filtrate to 6.0 by using an inorganic acid, cooling and filtering to obtain a crude product and mother liquor, washing the crude product by using water, ethanol and diethyl ether, and drying to obtain a finished product p-chlorophenylglycine; wherein the catalyst is trioctyl methyl ammonium chloride; wherein the molar ratio of the p-chlorobenzaldehyde to the trioctyl methyl ammonium chloride to the chloroform to the sodium hydroxide to the ammonium bicarbonate is 1.0 : (0.02-0.38) : (1.5-2.5) : (6.0-10.0) : (0.03-0.07). The synthesis process is simple, raw materials are easy to obtain,the reaction is milder, and toxicity and pollution of cyanide are avoided.

The invention relates to a synthetic method of 1-(4-chlorophenyl)-2-cyclopropyl-1-acetone. The synthetic method comprises the following specific steps: (1) dissolving p-chlorobenzaldehyde in an organic solvent, adding dialkyl phosphate, adding base at a certain temperature to carry out a catalytic reaction for a period of time; (2) continuously adding base after the catalytic reaction, dropwise adding cyclopropyl methyl ketone within a certain temperature range, reacting for a period of time, postprocessing, and distilling to obtain high-purity 1-(4-chlorophenyl)-2-cyclopropyl-1-acetone. The reaction equation is as shown in the specification. The method has the following advantages: the reaction steps are short; utilization rate of equipment is high; application amount of a solvent is small; production cost is low; the method is safe and environment friendly and is convenient to operate; the postprocessing mode is simple; purification is easy; and through distillation, 1-(4-chlorophenyl)-2-cyclopropyl-1-acetone with content being 97% and above is obtained.

The invention relates to a synthetic method of p-flurobenzaldehyde, which belongs to the chemical and pharmaceutical field. In the synthetic method, the p-chlorobenzaldehyde and potassium fluoride react under the condition of a solvent and a catalyst at high temperature, wherein, the solvent is one of sulfolane, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, hexamethyl phosphoramide, nitrobenzene and ortho-nitrotoluene; the catalyst is one of or the mixture of two or more than two of benzyl triethyl amine chloride, tetrabutylammonium bromide, hexadecyltrimethylammonium chloride, methyltrioctylammonium chloride, tetraphenylphosphonium bromide, methyltriphenylphosphonium bromide, benzyl triphenyl phosphonium bromide and polyethylene glycol dimethyl ether. Compared with the conventional preparation method, the synthetic method of the invention has the advantages of cheap raw materials, short synthetic route and little 'three wastes' discharge. As the amount of the catalyst used is reduced and the price of the solvent is low, the production cost of the p-flurobenzaldehyde is decreased.

The invention relates to a method for preparing a broad spectrum antibiotic of chloramphenicol. The method comprises the following steps of: synthesizing (1R,2R)-2-nitro-1-(4-chlorophenyl)-1,3-propanediol by using 4-chlorobenzaldehyde and 2-nitroethylalcohol as raw materials in the presence of a chiral catalyst, and performing catalytic hydrogenation to obtain (1R,2R)-2-amino-1-(4-chlorophenyl)-1,3-propanediol; and performing nitro substitution and dichloro acetylization on the intermediate to obtain the chloramphenicol. By the method, the common chiral resolution and aluminum isopropoxide reduction in the industry at present can be avoided, three wastes are reduced, the raw materials and reagents are cheap and readily available, p-chlorobenzaldehyde is selected as a raw material, the method comprises a few synthesizing steps, the yield is high, and the method is suitable for industrial production.

The invention discloses a preparation method of Metconazole, and the method comprises the following steps: carrying out water decarboxylation on a methylated product obtained by methylation of 2-methoxy acyl cyclopentanone to obtain 2-methyl cyclopentanone; reacting 2-methyl cyclopentanone with p-chlorobenzaldehyde to obtain 2-(4-chlorobenzylidene)-5-methyl cyclopentanone; carrying out methylationto obtain 5-(4-chlorobenzylidene)-2,2-dimethyl cyclopentanone; 5-(4-Chlorobenzylidene)-2,2-dimethylcyclopentanone undergoes Corey-Chaykovsky reaction to obtain an epoxide; reacts the epoxide with triazole to obtain a ring-opening product; and carrying out catalytic hydrogenation on the ring-opening product to obtain the Metconazole. The raw materials adopted by the preparation method are low in cost and easy to obtain in the market. The reactions in each step are conventional, the reaction steps are simple and easy to implement, and the method is simple process, mild in reaction conditions and easy in operation. The method has the advantages of high conversion rate, short reaction time and easy control, and is beneficial to industrial production.

The invention relates to a method for preparing p-chlorobenzaldehyde through continuous oxidization of p-chlorotoluene and belongs to the technical field of organic synthesis processes. The method is a process technology for preparing p-chlorobenzaldehyde by continuously oxidizing p-chlorotoluene in a tubular reactor with a p-chlorotoluene compound as a raw material, one or more metal ion complexes of cobalt, molybdenum and bromine as a catalyst, hydrogen peroxide as an oxidizing agent and acetic acid as a solvent. The method has mild conditions and takes short time, the utilization rate of the raw material is high, effective control in the reaction process can be realized, safe, stable and continuous operation is realized, and the production efficiency is high.

The invention discloses a synthetic method and applications of a modified polyaspartic acid with a Schiff base structure. The synthetic method comprises following steps: cis-butenedioic anhydride is introduced into a reactor containing distilled water, and is subjected to water bath stirring at 30 to 60 DEG C; ammonia water is introduced into the reactor drop by drop, and reaction is carried out for 0.5 to 3h at 60 to 100 DEG C; at argon atmosphere, oil bath treatment is adopted to increase the temperature to 180 to 240 DEG C, reaction is carried out for 20 to 40min, N, N-dimethyl formamide isadded for dissolving of a sticky substance, and product PSI is obtained via reaction; PSI and thiocarbazide are dissolved in a reactor containing distilled water, heating stirring is carried out for6 to 12h so as to obtain product PASP/CD; and at last the obtained PASP/CD aqueous solution and an alcoholic solution of p-chlorobenzaldehyde are subjected to heating backflow so as to obtain the modified polyaspartic acid with a Schiff base structure. The main chain of the modified polyaspartic acid corrosion inhibitor with a Schiff base structure is a biodegradable polymer, and the corrosion inhibition efficiency is 90% or higher.

The invention relates to a preparation method for a triticonazole intermediate 5-(4-chlorobenzylidene)-2,2-dimethylcyclopentanone. The preparation method comprises: (1) performing an oximation reaction on cyclopentanone and morpholine in an organic solvent in the presence of p-methylbenzene sulfonic acid at a temperature of 40-80 DEG C, so as to generate an intermediate I; (2) performing a condensation reaction on the intermediate I and p-chlorobenzaldehyde in a solvent at a temperature of 40-80 DEG C, so as to generate an intermediate II; (3) hydrolyzing the intermediate II under an acidic condition to generate an intermediate III; and (4) performing a methylation reaction on the intermediate III and a halogenated methane in a polar solvent in the presence of a strong base at a temperature of 40-80 DEG C, so as to generate 5-(4-chlorobenzylidene)-2,2-dimethylcyclopentanone. The technology is relatively simple, is capable of effectively controlling the impurity content in the product a improving the product impurity, and is low in cost and beneficial for realizing nationalization of triticonazole.

The invention relates to a synthetic method of cyproconazole intermediate. The synthetic route is as follow (see the formula in the description). The method includes the steps that p-chlorobenzaldehyde is used as a raw material, an acetal intermediate is obtained through condensation of p-chlorobenzaldehyde and ethylene glycol monomethyl ether, by means of triethyl phosphite, the acetal intermediate reacts with cyclopropyl methyl ketone under the alkaline condition, and finally the target compound (I) is obtained through hydrolysis. The synthetic method has the advantages of being safe, convenient, smooth in process and suitable for industrial production.

The invention discloses a green industrial production method of baclofen and belongs to the technical field of medicine synthesis. The method is carried out with p-chlorobenzaldehyde as an initial raw material and includes five reactions of Knoevenagel condensation, alkaline hydrolysis, imidation, alkaline hydrolysis, and Hofmann degradation, thus preparing the baclofen satisfying clinical medicinal application. The method employs raw materials being very easy to obtain and being low in cost and is simple in synthesis operations, wherein the reactions are carried out under aqueous conditions. The method is very low in environment pollution and high in yield, and is a novel industrial production method of the baclofen.

The invention provides a preparation method of p-chlorine methyl cinnamate, which comprises the following steps: taking basic ionic liquid 1-butyl-3-methylimidazole carbonate as a solvent and a catalyst, tetrabutyl ammonium bromide as a phase-transfer catalyst for stirring and mixing with methyl acetate under the temperature of 5 DGE C, then adding p-chlorine benzaldehyde for a condensation reaction, adding dilute sulfuric acid after the reaction, wherein the pH value of a reaction solution is between 6.5 and 7.2; filtering, wherein the obtained filtrate can be taken as a mixed liquid of ionic liquid and the phase-transfer catalyst; filtering the obtained solid, washing and drying to obtain p-chlorine methyl cinnamate. The method of the invention has the advantages of simple method, mild reaction condition, convenient operation, easy catalyst recovery and multitime repetitive usage; the product has the advantages of reliable and stable quality, high yield and no environmental pollution, and the method of the invention is a green synthetic method.

The invention discloses a method for preparing 4,4-dimethyl-1-(4-chlorphenyl)-3-pentanone, which comprises the following steps: reacting 3,3-dimethyl-2-butanone and p-chlorobenzaldehyde under reflux for 5-10 hours by using methanol as a solvent and sodium methoxide as an alkalizer, recycling part of methanol, cooling to 10-20 DEG C, filtering to obtain the 4,4-dimethyl-1-(4-chlorphenyl)-3-pentanone, and drying, wherein the mol ratio of p-chlorobenzaldehyde:3,3-dimethyl-2-butanone:sodium methoxide is 1:(1.0-1.3):(1.2-1.5). Methanol is substituted for potassium hydroxide, so that water generated in reaction is decomposed by sodium methoxide, thereby effectively enhancing the reaction speed and reaction yield; and since the reaction system does not contain water, the solvent can be recycled by simple distillation, thereby greatly lowering the facility request and reducing the raw material unit consumption. The synthesis yield of the method is higher than 97%, the product content is higher than 96%, and the recovery rate of the solvent methanol is up to 85%; and thus, the invention can easily implement industrial production, has good practicality, and can generate high economic benefit and social benefit.