22 results about "Chloroformate" patented technology

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 discloses a positive pole piece and a preparation method thereof, a diaphragm-free battery and a battery. The positive pole piece comprises a positive pole current collector and a positive pole active material layer arranged on at least one side of the positive pole current collector, the positive pole active material layer comprises a polymer, and the polymer is formed by polymerizing at least one of small molecules of the following raw material components: vinylethylene carbonate, vinylene carbonate, 2, 3, 4-trimethyl-1, 3-pentanedione, 2, 3, 4-trimethyl-1, 3-pentanedione and 2, 3, 4-trimethyl-1, 3-pentanedione. The adhesive is prepared from 2, 4-hexadienoic acid, allyl trifluoroacetate, diethyl allylmalonate, allyl methacrylate, allyl chloroformate, allyl phenylacetate, allyl acetate, allyl 4-hydroxybenzoate and allyl phenoxyacetate. The adhesive is prepared from the following raw materials: 1, 4-hexadienoic acid, allyl trifluoroacetate, diethyl allylmalonate, allyl methacrylate, allyl chloroformate, allyl phenylacetate, allyl acetate, allyl 4-hydroxybenzoate and allyl phenoxyacetate. The positive pole piece provided by the invention comprises the polymer, so that the interface impedance can be reduced, and the rate capability of the battery can be improved.

This invention belongs to the field of chloroformate synthesis technology, and particularly relates to a continuous preparation method of chloroformates, comprising the following steps: 1) feeding the reactant raw material alcohol and phosgene together into a synthesis tower via an absorption tower for reaction, generating crude chloroformate and byproduct hydrogen chloride; 2) sending the crude chloroformate formed in step 1) to a degassing tower, returning the phosgene removed from the degassing tower to the synthesis tower for further reaction, and then distilling the chloroformate after phosgene removal into a purification system to obtain the target product chloroformate; 3) sending the byproduct hydrogen chloride formed in step 1) into an absorption tower for washing with the raw material alcohol and then into the tail gas system. The beneficial effects of this invention are: it realizes continuous production of chloroformate products through synthesis and deacidification, improves the synthesis reaction rate, and shortens the deacidification time; simultaneously, through the recovery and recycling of phosgene, it reduces raw material consumption and forms a clean, inherently safe, automated production process.

The invention discloses anti-mildew plastic for a packaging container and a preparation method of the anti-mildew plastic, and relates to the technical field of plastic. The plastic is prepared from the modified biochar and the modified polyethylene; wherein 3, 5-diformylphenylboronic acid, 5-nitro-2-(oxiranyl methoxy) acetophenone, ethynyl magnesium bromide, isobutyldichlorosilane, hydroxylamine hydrochloride, ammonium salt and 3-butenyl chloroformate are used for synthesizing an anti-aging substance, then the anti-aging substance and polyethylene are subjected to cross-linking modification, an ultraviolet absorption group, a silicon-carbon bond and a boron-carbon bond are introduced into a polyethylene side chain, and the anti-aging substance is prepared. While the photo-thermal aging of the plastic is prevented, the barrier property of the plastic is improved; the biochar is modified by aminopropyl methyl dimethoxysilane, N, N-diethyl-p-aminobenzaldehyde, 11-chlorodecanoic acid and chitosan, antibacterial groups are generated on the surface of the biochar, and the biochar and modified polyethylene can be stacked in order, so that movement of water vapor and oxygen is prevented, and the anti-mildew effect of the plastic is improved.

The application relates to a synthesis method for constructing 2,4-imidazolidinedione compounds in a DNA coding compound library. The method takes 2-amino-N-acetamide compounds of On-DNA and p-nitrophenyl chloroformate as raw materials, reacts under the action of alkali, and obtains 2,4-imidazolidinedione compounds. The method has the advantages of mild reaction condition, simple operation, good substrate universality, good product yield and suitability for DNA coding compound synthesis in a multi-well plate.

The present application relates to the synthesis of pesticide compounds, in particular to a method for preparing a pyrasulfotole intermediate. The method comprises: (1) using p-chlorotoluene as a raw material, through nitration, chlorination, hydrolysis, or chlorination, hydrolysis, nitration, to obtain 3-nitro-4-chlorobenzaldehyde, (2) fluorination and reduction of 3-nitro-4-chlorobenzaldehyde to obtain 4-fluoro-3-amino benzaldehyde; (3) 4-fluoro-3-amino benzaldehyde is then contacted with chloroformate for reaction, and then chlorination to obtain compound IV; (4) compound IV is contacted with trifluorobutanamine ester under alkaline conditions for reaction to obtain compound I. The process for preparing compound I avoids using expensive raw material 2-chloro-4-fluorobenzoic acid, effectively reduces the cost of raw materials, reduces the three wastes generated in the process, and at the same time, the total yield of the reaction is high, and it is suitable for industrial mass production.

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 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.

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.

The utility model discloses an isooctyl chloroformate continuous production device, the device comprises a synthesis unit and a deacidification unit which are communicated through a pipeline, the synthesis unit comprises a photochemical tower, a tail gas condenser and a crude product buffer tank, the side part of the photochemical tower is provided with an isooctyl alcohol inlet, a liquid light inlet and a crude product outlet, the crude product outlet is connected with a crude product buffer tank through a pipeline, the bottom of the tail gas condenser is provided with a shared port of a tail gas inlet and a liquid-light outlet, and the liquid-light outlet is connected with a liquid-light inlet of the photochemical tower through a liquid-light backflow pipeline; the deacidification unit comprises a falling film evaporator, a gas-liquid separation tank and a finished product temporary storage tank, the top of the falling film evaporator is communicated with the crude product buffer tank through a pipeline, the lower side of the falling film evaporator is communicated with the gas-liquid separation tank through a pipeline, and the bottom of the falling film evaporator is communicated with the top of the finished product temporary storage tank through a pipeline. The device can realize continuous synthesis and deacidification of isooctyl chloroformate, and is low in phosgene consumption, high in product yield, safe and environment-friendly.

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.

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.

The invention discloses a method for detecting related substances in n-amyl chloroformate by a GC (Gas Chromatography) method, and belongs to the technical field of chemical engineering and pharmacy, the related substances in the n-amyl chloroformate are detected by a gas chromatography method, and temperature programming is adopted: the initial temperature is maintained for 18 minutes at 50 DEG C, the temperature is raised to 290 DEG C at 20 DEG C / min and maintained for 20 minutes, a constant flow mode is adopted, the flow rate is 2.0 ml / min, the split ratio is 10: 1, the temperature of a sample inlet is 200 DEG C, and the flow rate is 2.0 ml / min; the temperature of a hydrogen flame ionization detector is 290 DEG C, the content of 3-methylbutanol, 2-methylbutanol, n-amyl alcohol, 2-methylbutyl chloroformate and 3-methylbutyl chloroformate in n-amyl chloroformate can be effectively separated and quantitatively detected, and the method is simple and convenient to operate, high in specificity, high in sensitivity and accuracy, good in linearity, high in sensitivity and high in accuracy, and can be used for detecting the content of 3-methylbutanol, 2-methylbutanol, n-amyl alcohol, 2-methylbutyl chloroformate and 3-methylbutyl chloroformate in n-amyl chloroformate. And the quality of the n-amyl chloroformate product can be effectively controlled.

The invention provides a synthesis and purification process of high-purity chloroformate, and belongs to the technical field of chemical synthesis, and the synthesis and purification process comprises the following steps: S1, taking a mixed solution of bis (trichloromethyl) carbonate and an organic solvent as a base material, dropwise adding an alcohol compound under a temperature control condition, and carrying out phosgenation reaction to obtain a mixed reaction solution; s2, carrying out inert gas purging on the mixed reaction liquid obtained in the step S1 to remove free hydrogen chloride and phosgene so as to obtain a treated mixed liquid; s3, enabling the mixed solution treated in the step S2 to pass through an adsorption bed layer filled with an adsorption material, and carrying out deferrization and deacidification treatment; and S4, feeding the purified liquid obtained in the step S3 into a rectification unit, and separating the solvent from the product under a negative pressure condition to obtain high-purity chloroformate, the adsorption material comprises a zirconium-doped SBA-15 mesoporous molecular sieve skeleton, and an amidoxime group and a steric hindrance type tertiary amine group which are grafted on the surface of the skeleton. According to the process, the impurity content can be greatly reduced, and the product chromaticity index and the rectification yield can be improved.

The invention relates to oligomeric urea-amine molecules, preparation and application in carbon dioxide adsorption, and belongs to the technical field of high polymer materials. The preparation method comprises the following steps: firstly, reacting an amino-containing compound with p-nitrophenyl chloroformate to generate carbamate with a specific structure, and then reacting carbamate with hydrazine hydrate to combine amine groups in carbamate with hydrazine molecules in hydrazine hydrate to obtain oligomeric urea-amine molecules. The molecule has the characteristics of simple structure, excellent water solubility and high melting point, and can efficiently adsorb carbon dioxide; and after heating treatment at a relatively low temperature, desorption release of carbon dioxide can be realized, and regeneration of molecules can also be achieved.

The invention discloses a preparation method of tetradecyl chloroformate, which is characterized in that tetradecyl alcohol and phosgene are used as raw materials, tetradecyl chloroformate is used as a solvent, and tetradecyl chloroformate is prepared by reaction at the temperature of 0-30 DEG C. Compared with a conventional method, in the preparation method, by optimizing the solvent type and the reaction temperature condition, the reaction conversion rate and selectivity can be effectively improved, the technological process is simplified, high-yield and high-purity tetradecyl chloroformate can be rapidly and simply prepared, the product content is larger than or equal to 98%, the yield is larger 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 invention discloses a dopamine cationic lipid compound as well as a preparation method and application thereof, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: taking dopamine hydrochloride as an initial raw material, then carrying out a nucleophilic addition reaction with di-tert-butyl dicarbonate or tert-butyl chloroformate, and then reacting with 1-bromine halogenated hydrocarbon under an alkaline catalysis condition to obtain a dopamine derivative; and removing t-butyloxycarboryl on the dopamine derivative by trifluoroacetic acid, and reacting with halogenated hydrocarbon under an alkaline condition to obtain the dopamine cationic lipid compound. The dopamine cationic lipid compound prepared by the invention can enhance the intracellular delivery efficiency of bioactive molecules and therapeutic molecules, and a pharmaceutical preparation prepared by taking the dopamine cationic lipid compound as a delivery carrier can deliver the therapeutically effective dose of bioactive molecules to target cells, so that the dopamine cationic lipid compound has potential application value.

The present invention relates to the field of pesticides, and discloses a saflufenacil intermediate preparation method, which comprises: 1) carrying out a nitration reaction on a compound represented by a formula III, sulfuric acid and nitric acid to obtain a nitration product; 2) subjecting the nitration product to a hydrolysis reaction to obtain a compound of formula V; (3) carrying out hydrogenation reaction on the compound shown in the formula V to obtain a compound shown in a formula VI; (4) carrying out esterification reaction on the compound shown in the formula VI and chloroformate to obtain a compound shown in a formula VII; and (5) carrying out sulfonylation reaction on the compound as shown in the formula VII and N-methyl isopropylamine sulfonyl chloride to obtain a compound as shown in a formula VIII. The invention provides the novel preparation method of the saflufenacil intermediate, and the method is lower in cost, lower in three wastes and simpler to operate.

The application discloses an imiquimod prodrug and a preparation method and application thereof, and the structural formula of the imiquimod prodrug is shown in the following formula: the preparation method of the imiquimod prodrug comprises the following steps: step one, dissolving excessive imiquimod in anhydrous dioxane under a protective atmosphere, and dropping propargyl chloroformate dissolved in anhydrous dioxane under ice bath to obtain a mixture; step two, stirring the mixture obtained in the step one at 45-55 DEG C overnight; step three, filtering the product obtained in the step two, recovering excessive imiquimod, and purifying the filtrate after concentration and drying under reduced pressure to obtain the imiquimod prodrug. By using propargyloxy carbonyl to protect the amino group of the IMQ drug, the toxicity of the IMQ drug to cells is significantly reduced, and the systemic inflammatory response in mice is reduced; by using propargyloxy carbonyl to protect the amino group of the DOX drug, the toxicity of the DOX drug to cells is significantly reduced, and the cardiotoxicity in mice is reduced.

The invention relates to a process for preparing a carbonate compound (C), comprising: (a) reacting in a first reactor (V1), a first phenolic compound with phosgene in presence of a first solvent and sodium hydroxide, to obtain an intermediate product stream (P) comprising a chloroformate compound (CF); (b) passing the product stream (P) to a second reactor (V2) through a conduit, wherein the second reactor (V2) contains a reaction mixture (RM) comprising a second phenolic compound, a second solvent and a tertiary amine compound; and (c) reacting the second phenolic compound with the chloroformate compound (CF) to obtain the carbonate compound (C); wherein the product stream (P) upon formation, has a residence time of < 1.0 hour, in the first reactor (V1) prior to passing to the second reactor (V2).

The invention discloses a preparation method of [(5-thiazolyl) methyl]-(4-nitrophenyl) carbonate hydrochloride. The [(5-thiazolyl) methyl]-(4-nitrophenyl) carbonate hydrochloride is obtained by reacting 4-nitrophenyl chloroformate and 5-hydroxymethylthiazole under the catalysis of a pretreated supported K2O / Al2O3 catalyst. The catalyst can be recycled, the product selectivity is higher, the target product can be simply, conveniently and rapidly obtained through the preparation method, operation is easy and convenient, mother liquor can be recycled for multiple times, a large amount of waste liquid is not generated, the production cost is reduced, and industrial production is facilitated.