22 results about "Benzotrichloride" patented technology

The application discloses a continuous production process and equipment for a trifluoromethylbenzene tower, and belongs to the field of organic fluorine chemistry. The production process comprises the following steps: S1: continuously feeding trichloromethylbenzene and hydrogen fluoride into a tower reactor connected with a heat exchanger circulating cooling system in a reverse direction, so that a three-stage continuous fluorination reaction occurs in the tower reactor to obtain crude trifluoromethylbenzene, and unreacted hydrogen fluoride is separated into liquid at the top of the tower and then flows back into the tower reactor; S2: the crude trifluoromethylbenzene obtained in the reaction is subjected to nitrogen bubbling in a bubble tower, and then is continuously distilled in a rectifying tower to obtain finished trifluoromethylbenzene; and S3: byproduct hydrogen chloride generated in the fluorination reaction is introduced into a hydrochloric acid tank to obtain hydrochloric acid, and the content of hydrofluoric acid in the hydrochloric acid is less than 1000 ppm. The method can greatly improve the utilization rate of raw material hydrogen fluoride, improve the purity of byproduct hydrochloric acid, reduce the generation amount of waste acid, avoid the sharp change of pressure in the reaction process, and realize large-scale, continuous, stable and safe production of trifluoromethylbenzene.

The present application relates to the technical field of fine chemicals synthesis, and discloses a method for high-selectivity co-production of phthaloyl chloride and benzoyl chloride. The method uses dimethylbenzene and trichlorobenzene as raw materials, and feeds them into a photochlorination reaction tower to heat the materials. Then, the reaction tower is kept in a micro-negative pressure condition to perform photochlorination reaction. After the reaction is completed, the liquid is directly fed into a reaction kettle, and phthalic acid and a catalyst are added. Finally, the reaction liquid is separated by rectification to obtain the products phthaloyl chloride and benzoyl chloride. The present application greatly improves the selectivity of dimethylbenzene photochlorination reaction, and inhibits the ring chlorination side reaction. The present application can realize flexible co-production of m-phthaloyl chloride and p-phthaloyl chloride and benzoyl chloride, and can flexibly adjust the generation ratio of phthaloyl chloride and benzoyl chloride according to the raw material supply and product demand, thereby greatly improving the production flexibility of the reaction device.

The application belongs to the technical field of organic synthesis and particularly relates to a synthesis method of electronic-grade 2,3,4-trihydroxybenzophenone. The application comprises the following steps: catalytic reaction: taking water as a solvent, mixing water and a catalyst uniformly, adding pyrogallic acid, heating the system to 40-50 DEG C, continuously adding trichloromethylbenzene, performing insulation reaction, cooling the system to 10-15 DEG C after the reaction is completed, crystallizing and precipitating, and then filtering to obtain a crude wet product; purification treatment: removing impurities from the crude wet product to obtain the high-purity 2,3,4-trihydroxybenzophenone. The application does not need to react in an organic solvent system, is green and environmentally friendly, does not need nitrogen protection, has low production cost, and is suitable for industrialized processing and production, and the prepared 2,3,4-trihydroxybenzophenone has high purity and high yield.

The invention provides a synthesis method of L-acetoxypropionyl chloride, and belongs to the field of medical intermediates and fine chemical engineering. The preparation method comprises the following steps: mixing L-lactic acid and acetyl chloride for first reaction; then adding trichlorotoluene and a catalyst to carry out a second reaction; and then rectifying and separating to obtain the product L-acetoxypropionyl chloride. According to the method, two raw materials react to generate two products, no sulfur dioxide or acidic mixed waste gas is generated, the utilization rate of the raw materials reaches 100% theoretically, and the method completely conforms to an environment-friendly and pollution-free green process. The safety of the used trichlorotoluene is far higher than that of thionyl chloride and phosgene, the reaction is mild, the reaction speed can be controlled by controlling the temperature and the input amount of the catalyst, the production operation is relatively safe, and the purity of the prepared L-acetoxypropionyl chloride product is greater than 99%, and the yield is greater than 90%.

The invention belongs to the technical field of organic synthesis, and particularly relates to a green synthesis method of electronic-grade 2, 3, 4-trihydroxy benzophenone. The method comprises the following steps: catalytic reaction: taking water as a solvent, uniformly mixing water and a catalyst, adding pyrogallic acid, heating the system to 40-50 DEG C, continuously adding trichlorotoluene, carrying out heat preservation reaction, cooling to 10-15 DEG C after the reaction is completed, crystallizing, separating out and filtering to obtain a crude wet product; and purification treatment: removing impurities from the crude wet product to obtain the high-purity 2, 3, 4-trihydroxy benzophenone. The method does not need reaction in an organic solvent system, is green and environment-friendly, does not need nitrogen protection and is low in production cost, and the prepared 2, 3, 4-trihydroxy benzophenone is high in purity and yield and suitable for industrial processing production.

The utility model provides a heat exchange system for a reaction kettle and a reaction kettle for trichlorotoluene production, which belong to the technical field of reaction kettles and comprise a kettle body, a heat exchange sleeve, an air outlet pipe and an air blowing assembly. The heat exchange sleeve is fixedly sleeved outside the kettle body, and a heat exchange cavity is defined by the heat exchange sleeve and the kettle body. One end of the air outlet pipe is fixedly connected with the heat exchange sleeve and communicates with the heat exchange cavity. The air blowing assembly is fixedly connected with the heat exchange sleeve and comprises a cooling fan used for blowing air into the heat exchange cavity. According to the heat exchange system for the reaction kettle and the reaction kettle for trichlorotoluene production provided by the utility model, the cooling fan blows air into the heat exchange cavity, and air flow blown into the heat exchange cavity takes away heat on the kettle body and then flows out from the air outlet pipe, so that the cooling in the kettle body is accelerated, and the problem that the temperature in the kettle body is reduced slowly when the kettle body is cooled under natural conditions is avoided.

The present invention provides an improved process for the preparation of benzonitrile compounds More particularly, the present invention relates to an improved process for the preparation of benzonitrile compounds of Formula (I) by nitrilation of the corresponding benzotrichloride compounds of Formula (II).

The invention relates to a preparation process of 2-methyl-3-trifluoromethylaniline, which takes trichloromethyl benzene as a raw material and comprises the steps of nitration, fluorination, methylation and hydrogenation. According to the preparation technology, the trichloromethyl benzene raw material is cheap and easy to obtain, the synthesis steps are few, the yield can reach 90% or above, the selectivity can reach 99%, the purity of a finished product can reach 95% or above, and the production process is few in three wastes, environmentally friendly and suitable for industrial production.

The utility model discloses a tail gas absorption device in trichlorotoluene production, which belongs to the technical field of trichlorotoluene production, and comprises an absorption tank, the left side surface of the absorption tank is fixedly connected with a fixed plate, the left side surface of the fixed plate is fixedly connected with a filter cartridge, the right side surface of the absorption tank is fixedly connected with a support plate, and the support plate is fixedly connected with the filter cartridge. A liquid storage box is fixedly installed on the upper surface of the supporting plate, a liquid pump is fixedly installed on the upper surface of the liquid storage box, the output end of the liquid pump fixedly communicates with a liquid discharging pipe, and the end, away from the liquid pump, of the liquid discharging pipe penetrates through the absorption tank and extends into the absorption tank; and the end, away from the infusion pump, of the liquid drainage pipe fixedly communicates with a liquid drainage spraying disc, and the upper surface of the absorption tank fixedly communicates with a communicating pipe. According to the tail gas absorption device in trichlorotoluene production, organic matters and the like in tail gas can be physically adsorbed, the purpose of removing pollutants is achieved, the tail gas can be efficiently absorbed and treated, and the subsequent treatment requirement of the tail gas can be met.

The present invention relates to the technical field of organic synthesis, and discloses a method for synthesizing aromatic acyl chloride. In the present invention, carboxyl-modified quaternized cardanol is added to a reaction kettle at room temperature, and then anhydrous aluminum trichloride and benzotrichloride are added. Then, the temperature is slowly raised to 70-75 °C. After the reaction stops generating bubbles, the temperature is further raised to 105-110 °C and the reaction is carried out for 1-2 hours. After the reaction is completed, the reaction solution is transferred to a distillation flask and distilled to obtain aromatic acyl chloride. The aromatic acyl chloride of the present invention solves the problems of high energy consumption or introduction of other organic solvents, and at the same time has good antibacterial effects.

The present invention relates to the technical field of lithium ion battery electrolyte additive synthesis, and provides a method for preparing fluoroethylene carbonate. In the present invention, chloroethylene carbonate, a polymerization inhibitor, a catalyst, and liquid hydrogen fluoride are mixed to perform a fluorination reaction to obtain fluoroethylene carbonate. In the present invention, a polymerization inhibitor and a catalyst are added at the same time, thus the rate of reaction is increased, while avoiding the occurrence of side reactions such as material polymerization, thereby increasing the conversion rate and product yield. In the present invention, liquid hydrogen fluoride is used as a fluorination reagent, which is low in cost, easy to use, and convenient for continuous production. In the present invention, a trifluorotoluene compound is used as a solvent, and the trichlorotoluene compound is used to effectively utilize the remaining hydrogen fluoride, which is conducive to achieving full utilization of resources and reducing production costs. The fluorination reaction of the present invention can be carried out in a microchannel reactor, and can achieve continuous and automated production. In summary, the preparation method provided by the present invention is an efficient, economical, green, and environmentally friendly method with broad prospects.

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 3, 4-dichlorobenzotrifluoride, which comprises the following steps: firstly, adding dibenzoyl peroxide and N-hydroxyphthalimide into parachlorotoluene, and performing side chain chlorination reaction under ultraviolet irradiation and chlorine atmosphere to generate parachlorobenzotrifluoride; secondly, the obtained p-chlorobenzotrifluoride and tetrabutylammonium fluoride and potassium fluoride composite fluorination reagent are subjected to a fluorination reaction in the presence of a copper powder-1, 10-phenanthroline complex, and p-chlorobenzotrifluoride is prepared; and finally, under the catalysis of the mesoporous silica supported ferric trichloride catalyst, performing aromatic electrophilic chlorination on chlorobenzotrifluoride and sulfuryl chloride to obtain the high-purity 3, 4-dichlorobenzotrifluoride. Through synergistic application of photochemical chlorination, a composite fluorination system and the supported catalyst, the method has the advantages of mild reaction conditions, safe operation, high yield and good selectivity, and is suitable for industrial production.

The utility model relates to a benzoyl chloride continuous synthesis rectification production system which comprises a reaction kettle, the upper part of an outlet of the reaction kettle is connected with a distillation tower, the upper part of the distillation tower is provided with a condenser, and the middle part of the distillation tower and the top of the condenser are respectively communicated with a benzoyl chloride product collecting tank through pipelines; a gas-phase outlet of the condenser and a gas-phase outlet of the benzoyl chloride product collecting tank are respectively and sequentially communicated with the falling film absorption tower and the vacuum pump through pipelines; and the hydrochloric acid absorption tank circularly absorbs hydrogen chloride gas through a hydrochloric acid circulating pump to prepare hydrochloric acid. According to the method, trichlorotoluene and benzoic acid are used as raw materials, continuous heating, continuous feeding and continuous rectification are carried out in a vacuum state to obtain a finished product, a condensation reaction is carried out to generate a benzoyl chloride finished product, and hydrogen chloride gas generated by the reaction is continuously absorbed by water to prepare hydrochloric acid. The device disclosed by the utility model has the advantages of simple process route, high reaction speed, continuous production, one-step completion of synthesis and rectification, energy conservation, few preparation facilities and low emission of three wastes.

The invention provides a preparation method of 2-methyl-3-(trifluoromethyl) aniline and flunixin meglumine, which comprises the following steps: taking 3, 4, 5-trichlorotoluene as a raw material, and carrying out trichloromethylation reaction under the action of a first catalyst to obtain a trichloromethylation intermediate; carrying out halogen exchange reaction on the trichloromethylation intermediate under the action of a fluorinating agent to obtain a trifluoromethylation intermediate; carrying out nitration reaction on the trifluoromethylation intermediate under the action of a nitration reagent to obtain a nitration intermediate; and carrying out hydrogenation reduction reaction on the nitration intermediate under the action of a reducing agent and a second catalyst to obtain 2-methyl-3-(trifluoromethyl) aniline. According to the invention, 3, 4, 5-trichlorotoluene is taken as a starting raw material, the selectivity of trichloromethylation reaction is obviously improved, so that the yield of 2-methyl-3-(trifluoromethyl) aniline can be improved, and the method has the advantages of high selectivity, few byproducts, low cost and the like.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for separating and determining ibrutinib SM3 and impurities thereof based on gas chromatography. The impurities comprise any one or more of acrylic anhydride, trichlorotoluene, propionyl chloride, 3-chloropropionyl chloride, benzoyl chloride, acrylic acid and benzoic acid; the ibrutinib SM3 and impurities jointly form a composition to be detected. According to the method, (5% phenyl)-diphenylmethylsiloxane is adopted as a chromatographic column of a stationary liquid, or other stationary liquids with the same polarity are adopted; the ibrutinib SM3 and impurities of the ibrutinib SM3 are separated by adopting temperature programming; the temperature programming setting is as follows: the initial temperature is 35 + / -5 DEG C and is maintained for 5 + / -1 minutes, and the temperature is raised to 210 + / -10 DEG C at the rate of 30 + / -5 DEG C / min and is maintained for 8 + / -2 minutes. The method provided by the invention can effectively separate, identify and quantify various related substances in ibrutinib SM3, and has the advantages of short separation time, strong specificity, high sensitivity and good durability.

Methods of forming porous media (e.g., membranes for liquid separations or parts thereof) via polymerization, and related articles, are generally described. In some instances, two components are combined such that a polymerization (e.g., interfacial polymerization) reaction occurs, resulting in the formation of polymer layer (e.g., an active layer). In some instances, the two components include a first solution including water and a relatively low concentration of a first monomer (e.g., an amine-containing monomer such as optionally-substituted m-phenylenediamine) and a second solution including a nonpolar organic liquid and a relatively low concentration of a second monomer (e.g., an acid halide-containing monomer such as an optionally-substituted trimesoyl chloride).

The present invention discloses a synthetic method for an intermediate that can be used to prepare empagliflozin. Using o-chlorobenzotrichloride and fluorobenzene as starting materials, the production cost is reduced. During the reaction process, aluminum trichloride in the system is fully utilized, and a rare earth salt is used as an auxiliary catalyst to improve the selectivity of the reaction, reduce the impurities in the product, and at the same time, the synthetic process of the present invention also improves the product yield.

The present invention discloses an improved process for preparing a benzonitrile compound of formula (I) from the corresponding trichlorotoluene compound of formula (II).

The present invention relates to the field of chemical industry, and in particular to an environmentally friendly synthesis method for 4,4'-dimethoxytriphenylmethane. The synthesis route is as follows: #imgabs0# comprising the following steps: step 1, reacting anisole and trichlorotoluene in a polyethylene glycol solvent; step 2, recrystallizing the crude product to obtain pure 4,4'-dimethoxytriphenylmethane chloride. The present invention has the following beneficial effects: a one-pot synthesis of 4,4'-dimethoxytriphenylmethane is successful in a PEG-600 medium with high yield and good purity, which has significant advantages over previous methods; aluminum chloride produces more wastewater, causing environmental pollution. The use of PEG-600 avoids the use of aluminum chloride, thereby making the method environmentally friendly; treating aluminum chloride wastewater causes the production cost of 4,4'-dimethoxytriphenylmethane to increase. The use of PEG-600 and its ability to be reused at least five times significantly reduce the production cost of 4,4'-dimethoxytriphenylmethane.

The invention relates to the technical field of production of m-chlorobenzoic acid, in particular to m-chlorobenzoic acid and a preparation method thereof. The preparation method of the m-chlorobenzoic acid comprises the following preparation processes: under ultraviolet irradiation, mixing toluene and chlorine, and carrying out chlorination reaction to obtain trichlorotoluene; mixing trichlorotoluene, a sodium hydroxide solution and water, and carrying out hydration reaction to obtain sodium benzoate; mixing sodium benzoate with hydrochloric acid, and performing acidification reaction to obtain benzoic acid; the preparation method comprises the following steps: mixing benzoic acid, a sodium hydroxide solution and water, introducing chlorine, carrying out chlorination reaction, adding hydrochloric acid into the system, and acidifying to obtain m-chlorobenzoic acid. The preparation method provided by the invention has the advantages of clear process steps, easy control of reaction conditions of each step, easy operation, common equipment and low cost, and is suitable for large-scale continuous production.

The invention relates to a method and a device for industrially producing dichlorotoluene and application of a catalyst. The invention provides a method for industrially producing dichlorotoluene, which comprises the step of reacting m-chlorotoluene with chlorine in the presence of a catalyst, and the catalyst is a compound catalyst of a metal compound and a sulfur-containing compound. The main product of the reaction is 2, 5-dichlorotoluene, a small amount of byproducts are 3, 4-dichlorotoluene and 2, 3-dichlorotoluene, the primary reaction conversion rate of the raw materials is high, the main product 2, 5-dichlorotoluene is high in selectivity, and the byproduct trichlorotoluene is low. Wherein the catalyst is a compound catalyst of metal compounds such as aluminum, iron, nickel, titanium, copper, zirconium, antimony and the like and a sulfur-containing compound. According to the invention, a process for preparing 2, 5-dichlorotoluene, which is easy to industrialize, few in reaction steps, good in product directionality, high in yield and purity and low in production cost, can be provided.