19 results about "Chloroformic acid" 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 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.

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 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 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.

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.

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 discloses a preparation method and application of resveratrol prodrug-obeticholic acid nanoparticles, and the preparation method comprises the following steps: (1) dissolving resveratrol in an organic alkali and a solvent, dropwise adding an oxalyl chloride solution for reaction, then adding mPEG-OH for continuous stirring, after the reaction is finished, removing the solvent, and performing dialysis and freeze drying to obtain a Res prodrug polymer PRO; (2) PRO and OCA are dissolved in an organic solvent, deionized water is slowly added under stirring to achieve self-assembly, then PRO / OCANPs is obtained through dialysis, and the nanoparticles aim at specifically targeting tumor sites and are decomposed to release Res and OCA under the action of ROS in a tumor microenvironment, so that the treatment effect is achieved to the maximum extent.

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 invention provides an adamantane carbonate derived photoacid generator and a preparation method thereof.The method comprises the steps that triphosgene serves as a substrate, the triphosgene, adamantane methanol and organic alkali are dissolved in an organic solvent, after substitution reaction is conducted under the temperature control condition, reaction liquid is filtered and subjected to reduced pressure distillation, and a chloroformate adamantane methyl ester intermediate is obtained; the preparation method comprises the following steps: reacting an intermediate with 2-fluoro-2-bromoethanol and organic alkali in dichloromethane at a controlled temperature to obtain 1-adamantane methyl carbonate 2-bromo-2-fluoroethyl ester oily matter, sulfonating the oily matter to obtain a 1-adamantane methyl carbonate 2-fluoroethyl ester sodium sulfonate carbonate compound, and reacting the compound with 4-[1-(4-methoxybenzoyl)-2, 2, 4-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3 The preparation method comprises the following steps: carrying out anion exchange reaction on 2, 2-dimethylpropyl]-[1, 4] oxathietidine-4-onium trifluoroacetate in a mixed system of dichloromethane and water, concentrating an organic phase, and finally crystallizing isopropyl ether to obtain a target product.

The invention relates to the technical field of organic synthesis, in particular to a preparation process of peroxide 2-ethylhexyl tert-amyl carbonate with high active oxygen content. The invention overcomes the problems of low yield and low active oxygen content in the traditional method. The preparation method comprises the following steps: mixing tert-amyl hydroperoxide, a composite solvent, a modified catalyst and a free radical scavenger to construct a suspension system; under the conditions of low temperature and specific pH, dropwise adding chloroformic acid-2-ethylhexyl ester and the alkali salt solution to carry out interface directional reaction; and carrying out programmed heating and curing on the reaction liquid, filtering and recovering the modified catalyst, and chelating and washing to obtain a target product. Low-shear suspension is achieved through density matching of the composite solvent, reaction heat is effectively dispersed, and a modified catalyst is prevented from being broken; by utilizing the microenvironment regulation effect of the polyethylene glycol / quaternary ammonium salt double-modified resin, the hydrolysis side reaction is obviously inhibited, the obtained product is high in purity, and the process is safe.

The application belongs to the technical field of chemical engineering and specifically relates to a method for preparing di(2-ethylhexyl) peroxydicarbonate. The preparation method comprises the following steps: mixing potassium hydroxide solution and hydrogen peroxide to obtain reaction liquid A; adding a phase transfer catalyst to the reaction liquid A, and then mixing the reaction liquid A with chloroformic acid-2-ethylhexyl ester solution to obtain reaction liquid B; and cooling and washing the reaction liquid B to obtain di(2-ethylhexyl) peroxydicarbonate. The micro-channel reactor is used to continuously produce di(2-ethylhexyl) peroxydicarbonate. The reactants are reacted in multiple temperature zones, thereby breaking through the limitation of the reaction temperature (less than 44 DEG C). Di(2-ethylhexyl) peroxydicarbonate can be synthesized at high temperature, and the product has high yield, high purity and good reproducibility.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of tertiary butylperoxy-2-ethylhexyl carbonate with high active oxygen content. The invention overcomes the problems of low active oxygen content and low yield of the product in the prior art. The preparation method comprises the following steps: firstly, carrying out inclusion stabilization on tert-butyl hydroperoxide by using methyl-beta-cyclodextrin to construct a premixed solution; then introducing a modified catalyst into a composite solvent environment composed of isododecane and hydrofluoroether, and dropwise adding chloroformic acid-2-ethylhexyl ester through a low-temperature high-shear process to complete the reaction; and finally, carrying out solid-phase adsorption impurity removal by utilizing the modified hydrotalcite, and distilling to obtain the tert-butylperoxy-2-ethylhexyl carbonate. According to the method, interface heat and mass transfer is improved through the composite solvent, the reaction rate is increased through high-activity sites of the modified catalyst, anhydrous deacidification and dechlorination are achieved in cooperation with the modified hydrotalcite, raw material hydrolysis and peroxide bond thermal decomposition are effectively inhibited through the synergistic process, and the method has excellent industrial application value.