43 results about "Chloroformic acid" patented technology

The invention discloses a method for synthesizing alkyl carbonate through gas-phase carbonylation. Comprising a dechlorination method and a chlorine circulation process in the process of preparing alkyl carbonate through a gas-phase oxidative carbonylation reaction of carbon monoxide and alkyl nitrite. The content of water and alkyl alcohol in circulating gas is controlled through solvent absorption, alkyl chloride is synthesized with a chlorine supplementing agent HCl and alkyl chloroformate under the action of a dechlorinating agent, and the alkyl chloride is separated from a product through gas-liquid separation. When alkyl carbonate is produced by adopting the dechlorination method and the dechlorination process, the problem of equipment corrosion caused by chlorides can be avoided, the dechlorination process is a low-cost and environment-friendly chlorine circulation process, and stable operation of an industrial device is realized.

The invention provides a synthesis process of tert-amyl peroxy-2-ethylhexyl carbonate, and relates to the technical field of organic synthesis.The synthesis process comprises the following steps that S1, caustic soda liquid and water are pumped into a reaction kettle; s2, tert-amyl hydroperoxide is added into the reaction kettle for a salt forming reaction; s3, after the salt forming reaction is finished, adding a catalyst, dropwise adding isooctyl chloroformate, and carrying out condensation reaction to obtain a crude product of tert-amyl 2-ethylhexyl peroxide; and S4, carrying out alkali washing and water washing on the peroxide 2-ethylhexyl tert-amyl carbonate crude product to obtain a finished product. The catalyst is a tree-shaped structure catalyst of a silica gel carrier, and has the advantages of high conversion rate and high yield.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of diisopropyl peroxydicarbonate and application of the diisopropyl peroxydicarbonate. The preparation method comprises the following steps: firstly, adding isopropyl chloroformate and an ester-soluble organic solution into a three-necked flask, starting stirring, adding a hydrogen peroxide solution, slowly dropwise adding a sodium hydroxide solution into the three-necked flask when the temperature of a mixture in the flask is stabilized at-5 DEG C, controlling the time and temperature in the reaction process, finally separating out an organic phase, washing with water, and drying to obtain the isopropyl chloroformate. And drying with anhydrous sodium sulfate to obtain the product. According to the preparation method disclosed by the invention, by optimizing and precisely controlling the preparation process conditions, the preparation process is safe and controllable, the obtained diisopropyl peroxydicarbonate is high in yield and good in stability, can be directly used for preparing polyvinylidene fluoride, can be polymerized under a low-temperature condition without adding a chain transfer agent, improves the molecular chain regularity of polyvinylidene fluoride, has few abnormal structures, and is suitable for industrial production. The crystallinity is high, and the comprehensive performance is good.

The invention belongs to the technical field of organic peroxides, and particularly relates to a preparation method of peroxide (2-ethylhexyl) tert-amyl carbonate. The preparation method comprises the following steps: (1) carrying out temperature control reaction on a tert-amyl hydroperoxide crude product and a salt-forming agent under the action of a phase transfer agent to obtain an intermediate; (2) compounding a phase transfer catalyst system, blending the phase transfer catalyst system with chloroformic acid-2-ethylhexyl ester, adding the mixture and the intermediate into a reaction kettle for substitution reaction, and after the substitution reaction is finished, standing and collecting an upper organic phase to obtain a TAEC crude product; and (3) adding a detergent into the TAEC crude product, stirring, standing, collecting an upper oil phase, and washing until the oil phase is neutral to obtain TAEC. By compounding the phase transfer catalyst system, the problems of more dicarbonate byproducts, lower TAEC yield and difficulty in catalyst recovery in the existing TAEC synthesis method are solved.

The invention provides a method for preparing a telpotide side chain intermediate, which comprises the following steps: by taking 20-(tert-butoxy)-20-oxo-eicosanoic acid as a starting material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of 1-tert-butyl L-glutamic acid, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating and drying to obtain M2; taking M2 as a raw material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of AEEA-AEA, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating, and drying to obtain M4; and finally, taking M4 as a raw material, forming an active anhydride intermediate by using alkyl chloroformate, adding a strong alkali solution of Fmoc-lysine, reacting, adjusting the acid, extracting a product by using ethyl acetate, combining organic phases, concentrating, purifying, and drying to obtain the product. According to the method, amido bonds are formed in one pot, so that the purification process of the intermediate is reduced, the experimental steps are optimized, and the experimental cost is reduced.

The application belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of diisopropyl peroxydicarbonate and application of the diisopropyl peroxydicarbonate. The preparation method comprises the following steps: firstly, isopropyl chloroformate and an ester-soluble organic solution are added into a three-necked flask, stirring is started, hydrogen peroxide solution is added, when the temperature of the mixture in the flask is stabilized at-5 DEG C, sodium hydroxide solution is slowly added into the three-necked flask, and the time and temperature in the reaction process are controlled; finally, the organic phase is separated, washed with water, dried with anhydrous sodium sulfate, and obtained. The preparation method is safe and controllable, the yield of the diisopropyl peroxydicarbonate is high, the stability is good, the diisopropyl peroxydicarbonate can be directly used for the preparation of polyvinylidene fluoride, a chain transfer agent is not needed, polymerization can be carried out under low-temperature conditions, the molecular chain regularity of the polyvinylidene fluoride is improved, abnormal structures are few, the crystallinity is high, and the comprehensive performance is good.

The invention provides chiral 2, 15-dihydroxy tetrabenzocyclooctadiene and a preparation method thereof, and belongs to the technical field of organic compounds and synthesis. The method comprises the following steps: separating 2, 15-dihydroxy tetrabenzocyclooctadiene by utilizing a chiral preparative column through high performance liquid chromatography, and then confirming by utilizing a chiral reagent to obtain optical isomers (S)-2, 15-dihydroxy tetrabenzocyclooctadiene and (R)-2, 15-dihydroxy tetrabenzocyclooctadiene, namely, the (S)-2, 15-dihydroxy tetrabenzocyclooctadiene and the (R)-2, 15-dihydroxy tetrabenzocyclooctadiene and the (R)-2, 15-dihydroxy tetrabenzocyclooctadiene; the chiral reagent comprises one of (+)-(S)-10-camphor sulfonyl chloride, (-)-(R)-10-camphor sulfonyl chloride, (+)-menthyl chloroformate, (-)-menthyl chloroformate, (R)-(+)-alpha-methylbenzylamine and (S)-(-)-alpha-methylbenzylamine. The preparation method disclosed by the invention is simple, mild in reaction condition, easy to obtain reaction raw materials or precursors, convenient to separate and purify and high in yield, and has very practical value.

The invention relates to a phosgene purification method and a method for preparing chloroformic acid-2-ethyl ethyl. According to the method, the MOF material with excellent performance is prepared, and the MOF material is adopted to purify the phosgene, so that trace chlorine in the phosgene can be effectively removed, it is ensured that the chlorine is hardly contained in the phosgene, and adverse effects on downstream preparation of chloroformic acid-2-ethylhexyl ester are avoided. The invention also provides a method for preparing chloroformic acid-2-ethylhexyl ester, which comprises the step of reacting phosgene with isooctanol, and the phosgene is purified by the phosgene purification method. The method provided by the invention can reduce side reactions during preparation of chloroformic acid-2-ethyl ethyl, improve product purity and ensure product chromaticity.

The invention relates to the technical field of detection, and particularly discloses a method for detecting 2-aminothiazole in marine sediments in a sea area near an offshore wind field, which comprises the following steps: extracting a sample by using a mixed solution, then deriving by using hexyl chloroformate, converting a target compound 2-aminothiazole into N-(thiazole-2-yl) carbamic acid n-hexyl ester, and detecting the 2-aminothiazole in the marine sediments in the sea area near the offshore wind field by using the N-(thiazole-2-yl) carbamic acid n-hexyl ester. And enriching and purifying the obtained derivative by using a solid-phase extraction small column, and detecting by using a liquid chromatography-mass spectrometry system. The method provided by the invention can be used for efficiently, quickly and accurately analyzing and detecting, and is suitable for detecting 2-aminothiazole in marine sediments.

This invention belongs to the field of peroxide preparation technology, specifically relating to a heat exchange device and method for preparing peroxides. The heat exchange device includes heat exchange tubes disposed within a reaction vessel, with several heat exchangers mounted on the heat exchange tubes. Each heat exchanger includes several external fins spaced apart on a fixed plate. The fixed plate has grooves that mate with the heat exchange tubes, and the heat exchange tubes are disposed within these grooves. The peroxide preparation method involves stirring a desensitizer, a catalyst, and an oxidant together, followed by the addition of an alkyl acyl chloride or an alkyl chloroformate to continue the reaction. After the reaction is complete, a crude product is obtained. The crude product is then washed and separated to obtain the peroxide. This invention utilizes the high-efficiency heat transfer performance of the heat exchanger, thereby enabling stable preparation of peroxide products, reducing the reaction time, and improving the conversion efficiency from initial raw materials to peroxide products.

According to the technical scheme, the preparation method comprises the following steps: (1) taking 10-DAB as a raw material, and carrying out 10-site acetylation to obtain an intermediate I; (2) dissolving the intermediate I in dichloromethane, adding pyridine for dissolving, dropwise adding chloroformic acid-2, 2, 2-trichloroethyl ester, and reacting to obtain an intermediate II; (3) dissolving the intermediate II in methylbenzene, adding (4S, 5R)-2, 4-diphenyl-4, 5-dihydrooxazole-5-carboxylic acid and 4-dimethylaminopyridine, adding a condensing agent, and reacting to obtain an intermediate III; and (4) dissolving the intermediate III in tetrahydrofuran or acetone, adding acid, stirring to react, adding alkali after the reaction is finished, and continuously reacting to obtain the 7-trichloroethoxycarbonyl paclitaxel. The synthesis method is simple, reaction conditions are easy to control, each step does not need column chromatography, the product with the purity of more than 99% can be obtained by recrystallizing the crude product, the operation links are reduced, the production cost is saved, and the method is very suitable for industrial production.

The invention relates to the technical field of analysis and detection, and discloses a method for detecting ethanolamine in a Nicodil bulk drug, which comprises the following specific steps: (1) carrying out derivatization reaction on ethanolamine in the Nicodil bulk drug by using 9-fluorenylmethyl chloroformate as a derivatization reagent to obtain a sample containing an ethanolamine derivatization product; and (2) preparing a test solution from the sample containing the ethanolamine derivatization product, and detecting the test solution by high performance liquid chromatography. According to the method, the chloroformic acid-9-fluorenylmethyl ester is used as a derivatization reagent, the pre-column derivatization HPLC method is established to measure the ethanolamine in the Nicodil bulk drug by optimizing derivatization conditions and methodology verification, the conditions are mild, the operation is simple, and the sensitivity is high.

The invention discloses a preparation method of dodecyl chloroformate, which comprises the following steps: heating dodecanol to melt the dodecanol into a liquid state, introducing phosgene for reaction, reducing the reaction temperature to 0-20 DEG C in the reaction process, continuing the reaction until the content of the dodecanol in the reaction system is less than 0.5%, stopping introducing the phosgene, and keeping the temperature to obtain a reaction liquid; and heating the reaction liquid to 30 DEG C or above, introducing nitrogen, and removing impurities in the reaction liquid to obtain dodecyl chloroformate. Compared with the conventional method, the preparation method of dodecyl chloroformate can effectively improve the reaction conversion rate and selectivity by optimizing the reaction temperature of each stage in the reaction process, and can quickly and simply prepare high-yield and high-purity dodecyl chloroformate, the content is greater than or equal to 98%, the yield is greater than or equal to 98%, the product competitiveness can be improved, and the method is suitable for industrial production. The industrial application is convenient to realize and the industrial practicability is high.

The present application belongs to the technical field of organic synthesis, and particularly relates to a method and system for preparing diisopropyl peroxydicarbonate based on a micro-channel reactor. The present application uses a heart-shaped micro-channel reactor, pumps raw material potassium hydroxide solution and hydrogen peroxide solution from the inlet of the first piece, and pumps raw material isopropyl chloroformate from the inlet of the fourth piece, thereby realizing safe production in the preparation process of diisopropyl peroxydicarbonate, stable operation of the reaction, a substantial reduction in reaction time, accurate control of reaction temperature by a high-low temperature all-in-one machine, timely removal of heat, reduction in side reactions, a substantial increase in product yield, and finally obtaining a product with a yield of 99.5%, realizing source reduction in the preparation process, a reduction in energy consumption and raw material consumption per unit product, and fully meeting the strategic orientation of national green chemical industry and clean production. Meanwhile, the method of the present application can significantly reduce production cost, fill in the technical gap, enhance market competitiveness, and can be widely promoted.

The application discloses a method for continuously synthesizing isooctyl chloroformate, which comprises the following steps: preparing a continuous reaction device which comprises a photochemical tower, a transfer kettle and a chase light tower which are communicated with each other, feeding isooctanol and phosgene into the photochemical tower to perform a reaction, overflowing the obtained esterification liquid to the transfer kettle, performing gas-liquid separation on the obtained tail gas outside the tower, and feeding the liquid light into the tower; controlling the temperature of the transfer kettle at 30-40 DEG C, feeding the esterification liquid into the chase light tower after the transfer kettle collects a certain amount of esterification liquid, controlling the temperature of the chase light tower at 40-80 DEG C, feeding nitrogen into the chase light tower to perform chase light, and collecting high-purity isooctyl chloroformate in the chase light tower, wherein the content of the isooctyl chloroformate is greater than or equal to 99%, and the yield is greater than or equal to 97%. The method realizes continuous production under the premise of ensuring the quality and yield of the product, has small production land occupation, small liquid holdup of the reaction system, small risk, high production efficiency, easily controlled process conditions, little waste, accords with the green and environmental protection production concept, and is suitable for industrial production.

The present invention belongs to the technical field of organic peroxides, and particularly relates to a preparation method of tert-amyl peroxy (2-ethylhexyl) carbonate. The preparation method comprises the following steps: (1) carrying out a temperature-controlled reaction on a crude product of tert-amyl hydroperoxide and a salifying agent under the action of a phase transfer agent to obtain an intermediate; (2) compounding a phase transfer catalyst system, blending the phase transfer catalyst system with 2-ethylhexyl chloroformate, and adding the blend and the intermediate into a reaction kettle in a co-current manner to carry out a substitution reaction. After the substitution reaction is completed, standing and collecting the upper organic phase to obtain a crude TAEC product; (3) adding a detergent to the crude TAEC product, stirring, standing, collecting the upper oil phase, and washing with water until the oil phase is neutral to obtain TAEC. By compounding the phase transfer catalyst system, the present invention solves the problems of many by-products of dicarbonates, low yield of TAEC and difficult catalyst recovery existing in the current TAEC synthesis method.

The invention discloses a preparation method of 1, 1, 2, 2, 3, 3, 4, 4, 4-nonafluorobutane-1-sulfonic acid (2-hydroxyethyl)-amide, which comprises the following steps: (1) under the action of an acid-binding agent, perfluorobutyl sulfonamide and chloroformic acid-2-chloroethyl ester are subjected to acylation reaction in an organic solvent, and after the reaction is finished, the temperature is raised for cyclization reaction to obtain an intermediate reaction solution; and (2) adding water into the intermediate reaction solution obtained in the step (1), carrying out a hydrolysis decarboxylation reaction, and after the reaction is finished, carrying out post-treatment to obtain the 1, 1, 2, 2, 3, 3, 4, 4, 4-nonafluorobutane-1-sulfonic acid (2-hydroxyethyl)-amide. The preparation method has the advantages of cheap and easily available raw materials, simple route, mild conditions and environmental friendliness, the obtained product has good purity and high yield, and the method is more suitable for industrial production.

The invention belongs to the technical field of peroxide preparation, and particularly relates to a heat exchange device for peroxide preparation and a peroxide preparation method.The heat exchange device for peroxide preparation comprises a heat exchange pipe arranged in a reaction kettle, a plurality of heat exchangers are arranged on the heat exchange pipe, and each heat exchanger comprises a plurality of external fins; the external fins are arranged on the fixing plate at intervals, the fixing plate is provided with grooves matched with the heat exchange tubes, and the heat exchange tubes are arranged in the grooves of the fixing plate. The preparation method of the peroxide comprises the following steps: stirring a desensitizer, a catalyst and an oxidant for reaction, then adding alkyl acyl chloride or alkyl chloroformate for continuous reaction, and obtaining a crude product after the reaction is finished; and washing and separating the crude product to obtain the peroxide. The high-efficiency heat transfer performance can be realized by utilizing the heat exchanger, so that the peroxide product can be stably prepared, the charging reaction time is shortened, and the conversion efficiency from the initial raw material to the peroxide product is improved.

The invention belongs to the technical field of bacteria detection, and discloses an analysis method for detecting colistin in bacteria. The method comprises the following steps: firstly, centrifugally washing bacterial suspension incubated by sub-bacteriostasis colistin, and repeatedly freezing and thawing by adopting liquid nitrogen, so that bacterial cells are cracked; placing the split thalli in an acidic solution, and hydrolyzing at 60-120 DEG C in a protective atmosphere to obtain 2, 4-diaminobutyric acid; adjusting the pH to be neutral by using an alkaline solution to obtain hydrolysate; adding a derivatization buffer solution and a derivatization agent chloroformic acid-9-fluorenyl methyl ester into the hydrolysate, reacting at 20-80 DEG C to obtain a derivatization reaction solution, and treating to obtain filtrate; and separating the filtrate through a C8 reversed-phase chromatographic column, determining by selecting a fluorescence detector, and qualitatively and quantitatively analyzing the colistin in the bacteria by adopting a standard addition method, so that the colistin in the bacteria can be detected. According to the method, the colistin in the bacteria is detected by using a high performance liquid chromatography-fluorescence method, and a technical support is provided for exploring an antibacterial action mechanism of the colistin and a drug resistance mechanism of the bacteria.

The invention discloses hydroxycarboxylic acid-menthol carbonate as well as a synthesis method and application thereof, dimethyl malate and menthyl chloroformate are taken as raw materials, and malic acid monomethyl ester-menthol carbonate and malic acid-menthol carbonate are obtained through esterification and enzyme hydrolysis two-step reaction; dimethyl tartrate and menthyl chloroformate are used as raw materials, monomethyl tartrate-menthol carbonate is obtained through esterification and enzyme hydrolysis two-step reaction, dibenzyl tartrate and menthyl chloroformate are used as raw materials, tartaric acid-menthol carbonate is obtained through esterification and palladium carbon hydrolysis two-step reaction, and the operation method is simple and convenient. Hydroxycarboxylic acid-menthol carbonate is stable and non-volatile at room temperature, can be cracked to release menthol at the working temperature of cigarettes after being added to the cigarettes, can be efficiently cracked to release menthol at the temperature of 150-300 DEG C, and is suitable for heating the cigarettes, products released by malic acid-menthol carbonate at the high temperature mainly comprise menthol, the generated menthene is less, and the safety of the cigarettes is improved. The method is suitable for traditional cigarettes.

The application discloses a spiromesifen derivative, belongs to the field of crop disease and pest control, and has the structure shown in the following formula 1001, a preparation method thereof is as follows: under the protection of inert gas, 3-(2, 4, 6-trimethylphenyl)-2-oxo-1-oxaspiro[4, 5]-non-3-ene-4-ol and dichloromethane are stirred and cooled to 0-5 DEG C, then triethylamine is added, fluorine ethyl chloroformate is added dropwise, after dropwise addition is completed, the reaction is continued after being raised to room temperature, and then purification is conducted, and the spiromesifen derivative is obtained; the spiromesifen derivative has higher safety for citrus, watermelon and Chinese rose and has better pest control activity than that of spiromesifen.

The invention belongs to the field of organic matter preparation, and particularly relates to a preparation method of 9-fluorenyl methyl-N-succinimido carbonic ester, which comprises the following steps: dissolving N-hydroxysuccinimide, mixing with dried chloroformic acid-9-fluorenyl methyl ester and silicon-based solid alkali to react, quenching and washing after the reaction is completed, drying and purifying to obtain the 9-fluorenyl methyl-N-succinimido carbonic ester. The 9-fluorenyl methyl-N-succinimido carbonic ester is subjected to a reaction to obtain 9- The solid alkali is doped with ester groups. According to the method, the high-quality and high-purity product can be obtained, the requirement of a high-precision experiment for the product purity can be met, and the method is easy to operate and suitable for industrial popularization.

The application belongs to the field of organic matter preparation, and particularly relates to a preparation method of 9-fluorenylmethyl-N-succinimidyl carbonate, wherein N-hydroxy succinimide is dissolved and mixed with dry chloroformate-9-fluorenylmethyl ester and a silicon-based solid base for reaction, water is used for quenching and washing after the reaction is completed, and 9-fluorenylmethyl-N-succinimidyl carbonate is obtained after drying and purification; an ester group is doped on the solid base. The method can obtain high-quality and high-purity products, can meet the demand of high-precision experiments on product purity, and is simple to operate and suitable for industrial promotion.

The utility model relates to an air inducing device for isooctyl chloroformate tail gas treatment, which comprises a tail gas discharge header pipe, two groups of pre-treatment mechanisms, a middle pipe, two groups of air inducing mechanisms and a tail gas conveying header pipe, two first branch pipes are connected in parallel to the tail end of the tail gas discharge header pipe, two second branch pipes are connected in parallel to the head end of the middle pipe, and two third branch pipes are connected in parallel to the tail end of the middle pipe. The front treatment mechanism comprises an absorption tank, the absorption tank is divided into a first absorption chamber and a second absorption chamber through a partition plate, the two first branch pipes are in one-to-one correspondence with the two first absorption chambers, and the tail ends of the first branch pipes extend into the lower portions of the corresponding first absorption chambers; the first absorption chambers are communicated with the second absorption chambers in the same group through inverted U-shaped pipes, the two second branch pipes are in one-to-one correspondence with the two second absorption chambers, and the head ends of the second branch pipes extend into the upper parts of the corresponding second absorption chambers. According to the utility model, the damage to the induced draft fan can be reduced by pre-treating the tail gas, and the whole device is more flexible and convenient to use.

The invention provides a synthetic method of di (2-ethylhexyl) peroxydicarbonate and equipment for implementing the synthetic method. The synthesis method comprises the following steps that an alkaline solution, a hydrogen peroxide solution and a chloroformic acid-2-ethylhexyl ester solution are subjected to a primary reaction through a microreactor, a first oil-water mixed solution is obtained, and before the primary reaction, the alkaline solution, the hydrogen peroxide solution and the chloroformic acid-2-ethylhexyl ester solution are mixed through a micromixer; conveying the first oil-water mixed solution into an aging reaction kettle for continuous reaction to obtain a second oil-water mixed solution; performing liquid separation treatment on the second oil-water mixed liquid to obtain an oil phase; and carrying out post-treatment on the oil phase to obtain the di (2-ethylhexyl) peroxydicarbonate. The active oxygen content of the di (2-ethylhexyl) peroxydicarbonate obtained by the synthesis method disclosed by the invention reaches 4.61%, and the chlorine content is lower than 0.05%.

This invention belongs to the field of organic synthesis technology and relates to a method for preparing (S)-4-(2,4-difluorophenyl)-2-(hydroxymethyl)pent-4-en-1-yl isobutyrate. 2,4-Difluoroiodobenzene reacts sequentially with allyl alcohol and tert-butyl chloroformate to obtain 2-(2,4-difluorophenyl)allyl tert-butyl carbonate. Under the action of a palladium catalyst and Sadphos chiral phosphine ligand, the 2-(2,4-difluorophenyl)allyl tert-butyl carbonate undergoes alkylation and reduction to obtain (S)-4-(2,4-difluorophenyl)-2-(hydroxymethyl)pent-4-en-1-yl isobutyrate. This invention utilizes a palladium catalyst and Sadphos chiral phosphine ligand to precisely construct a chiral center in one step, achieving an enantioselectivity of up to 99.4% and an overall yield of 65-70%. The operation is simple, the catalyst is recyclable, significantly reducing production costs and making it suitable for industrial production.

This application relates to the technical field of organic light-emitting materials, and particularly to a chiral light-emitting molecule and its preparation method, as well as a chiral light-emitting liquid crystal. The preparation method of the chiral light-emitting molecule includes the following steps: S1: Menthyl chloroformate, 4-phenol-2,1,3-benzothiadiazole, palladium catalyst, and acid-binding agent are sequentially added to a flask, followed by the addition of an organic solvent for dissolution and thorough stirring to obtain a mixture; S2: The mixture is injected into a nitrogen-filled reaction vessel, heated to 70–95°C, reacted for 5–10 hours, and then separated and purified to obtain the chiral light-emitting molecule. Compared with traditional preparation methods such as alkylation, acylation, dehydration, and ring-opening methods, the preparation method of this application significantly shortens the reaction time while increasing the yield; furthermore, this method is simple to operate, the reaction is mild, and it can be carried out under conventional laboratory conditions, reducing the cost of chiral light-emitting molecules.

The reaction kettle structure comprises a kettle body, a liquid pump is arranged at the outer top of the kettle body, an air pump is arranged at the outer bottom of the kettle body, a liquid inlet of the liquid pump is communicated with a liquid conveying pipeline, a liquid outlet of the liquid pump is communicated with a liquid inlet pipe, and the tail end of the liquid inlet pipe downwards extends into the kettle body and is rotationally connected with a liquid spraying pipe. The peripheral side of the lower part of the liquid spraying pipe is communicated with a plurality of liquid spraying branch pipes, the bottom ends of the liquid spraying pipe and the liquid spraying branch pipes are communicated with liquid spraying nozzles, an air inlet of the air pump is communicated with an air conveying pipeline, an air outlet of the air pump is communicated with an air inlet pipe, and the tail end of the air inlet pipe upwards extends into the kettle body and is rotationally connected with an air spraying pipe; a guide rail is arranged on the top in the kettle body, an electric sliding block is arranged on the guide rail in a sliding mode, the bottom end of the electric sliding block is fixedly connected with an L-shaped connecting rod, and the tail end of the connecting rod is fixedly connected with a rotating frame. According to the utility model, the hedging contact of alcohol and phosgene and efficient and high-quality stirring can be realized, and the reaction efficiency and quality are higher.

This invention belongs to the field of compound synthesis technology, specifically relating to a method for synthesizing biphenylhydrazine, comprising the following steps: (1) mixing isopropyl chloroformate and hydroxylamine hydrochloride in solvent a, and reacting under certain temperature and alkaline conditions to obtain intermediate 1; (2) mixing intermediate 1 with a hydrocarbon sulfonyl halide in solvent b, and reacting under certain temperature and alkaline conditions to obtain intermediate 2; (3) mixing intermediate 2 with 3-amino-4-methoxybiphenyl in solvent c, and reacting under certain temperature and alkaline conditions to obtain biphenylhydrazine. This invention provides a novel method for synthesizing biphenylhydrazine. The synthesis of biphenylhydrazine in this application uses new raw materials and intermediates, which has the advantages of inexpensive raw materials, short synthesis route, mild reaction conditions, high yield, and ease of industrial production.

A system and method of making a silylcarbonate compound, the method including reacting trialkylsilylalcohol with alkyl chloroformate in the presence of a base at an elevated temperature to form the silylcarbonate compound.