23results about "Preparation by halogen introduction" patented technology

Provided is a method for producing an organohalogen compound with which it is possible to produce an organohalogen compound with high selectivity and high yield. A method for producing an organohalogen compound, which comprises a halogenation step for obtaining an organohalogen compound (A) represented by formula (1) by halogenating a compound represented by formula (1 [alpha]) as a starting material, the halogenation step being a step for halogenating in a multiphase-containing system, the plurality of phases include an organic phase containing an organic solvent as a solvent and an aqueous phase containing water as a solvent.

To provide a new method for producing a fluorinated organic compound in which removal or separation of an auxiliary is easy and which is advantageous in production cost.SOLUTION: A compound represented by the following formula (1): wherein R1, R2 and n are as defined in the description. The method comprises reacting the compound represented by the formula (1) with (A) at least one fluorine source selected from hydrogen fluoride, a hydrogen fluoride salt and a fluoride salt, (B) at least one iodine source selected from iodine and ammonium iodide, and (C) a compound having at least one fluorinated quaternary nitrogen atom in the molecule. A step of difluorinating the compound represented by the formula (1), wherein the amount of the iodine source (B) used is less than 1.0 mol per 1 mol of the compound represented by the formula (1).SELECTED DRAWING: None

The invention discloses a preparation method of high-purity 2-fluoroethanol, and particularly relates to the technical field of preparation of 2-fluoroethanol, which comprises the following steps: S1, in a dual-catalyst system consisting of a phase transfer catalyst and a Lewis acid catalyst and an organic solvent, carrying out fluoridation reaction on 2-chloroethanol and anhydrous potassium fluoride at 60-120 DEG C for 2-10 hours to obtain 2-chloroethanol; and S2, sequentially carrying out integrated purification of filtration, reduced pressure distillation, adsorption treatment and rectification on the reaction mixture. According to the invention, through synergistic activation and mass transfer of double catalysts, the reaction rate and selectivity are significantly improved, the water segregator is utilized to remove reaction water to push equilibrium movement, the conversion rate is improved, and water and impurities are systematically removed by virtue of composite adsorption and precise rectification of molecular sieves and activated carbon, so that high-quality 2-fluoroethanol with high purity and low moisture is finally obtained. The whole preparation process is mild in condition, high in yield, good in safety and suitable for industrial production.

The utility model relates to the technical field of preparation of dichloropropanol from glycerol, in particular to a production system for producing dichloropropanol through glycerol chlorination. The device comprises an adipaldehyde mixing tank for mixing adipaldehyde and pure water, a gas-liquid reaction kettle for absorbing chlorine in crude hydrogen chloride, a first microporous filter for filtering out a catalyst, a cooler for cooling crystals and a second microporous filter for removing crystals. The method has the effects of improving the problem of side reaction caused by chlorine impurities in crude hydrogen chloride and increasing the conversion rate of glycerol.

The application discloses a method for constructing fluorine-containing compounds by decarboxylation of alkyl carboxylic acid catalyzed by ketone compounds. The method uses alkyl carboxylic acid with a structure as shown in formula as a reaction raw material, and performs reaction under the joint action of ketone compounds, fluorine-containing reagents and alkali to obtain fluorides shown in formula (1) and formula (2), wherein R 1 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl; R 2 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl; R 3 are respectively and independently selected from hydrogen, a heterocyclic ring, substituted or unsubstituted aryl, and substituted or unsubstituted hydrocarbyl. The reaction method has the advantages of low cost, mild conditions, high reaction efficiency, high yield and high selectivity, and the like. The ketone compounds are used to replace traditional metal catalysts, which can not only provide a fluorine-containing compound library with various structures for candidate drug screening, but also can be applied to positron emission tomography imaging.

The application provides a preparation method and a production system for preparing dichloropropanol by glycerol chlorination, and belongs to the technical field of compound preparation. The method adopts multistage series connection of reaction kettles for reaction, and precisely controls the chlorination reaction process by controlling the reaction temperature and the dehydration amount. In the reaction, hydrogen chloride gas is kept in communication with all the reactors, glycerol and a catalyst are fed into a first-stage reaction kettle for reaction, liquid-phase products are transferred into a next-stage reaction kettle for continuous reaction, and gas-phase products are transferred into the original reaction kettle for continuous reaction after dehydration. The method provided by the application can not only precisely and efficiently solve the water inhibition problem in the reaction process, but also can improve the chlorination reaction efficiency, the selectivity and the yield of dichloropropanol, and the purity of the product.

Process for the hydrochlorination of alkenes, comprising the following steps: a)- preparing an organic solution A of a compound (I) comprising at least one alkene function by dissolving it potentially in an organic solvent; b)- mixing the solution A with a aqueous solution B comprising hydrochloric acid; c)- stirring the mixture comprising solution A and solution B at stirring speed of at least 500 rpm, and at a temperature in the range from -5 to 105°C for at least half an hour.

The application provides a production process and device and application thereof for co-production of 3-chloropropylene and dichloropropanol, comprising: allowing raw materials of propylene and chlorine to occur halogenation reaction in a halogenation reactor, and allowing the halogenation reaction product to enter a heat exchanger, and after heat exchange, the halogenation reaction product is divided into a gas phase part and a liquid phase part, wherein hydrogen chloride gas in the gas phase part is used as raw material to occur hydrochlorination reaction with glycerol and a catalyst in a hydrochlorination reactor, and is used for preparing dichloropropanol; and the liquid phase part enters a rectifying column to separate and purify to obtain 3-chloropropylene, the application fully utilizes a large amount of hydrogen chloride by-produced in a high-temperature chlorination process of propylene, and supplies a chlorine source required in a glycerol hydrochlorination process, so that a by-production recovery treatment process in the high-temperature chlorination process of propylene is omitted, a production process is simplified, energy consumption is reduced, the device is simple to operate, equipment production efficiency is high, and industrial application is facilitated.

A formulation for forming a flame-retardant polyurethane is provided. 【Solution means】A formulation containing a compound of formula I and at least one polyol is provided. TIFF2026065142000023.tif44165 Wherein, X 1 and X 2 are each independently H, Cl, or Br, and at least one of X 1 or X 2 is Br; R 1 is H, Cl, Br, C1-C4 alkyl, etc.; R 2 is H or C2-C8 alkyl hydroxyl; R 3 and R 4 are each independently H, C1-C8 alkyl, C2-C8 alkenyl, C1-C8 haloalkyl or C2-C8 haloalkenyl; n = 1 to 4; m = 1 to 4.

Provided is a novel method for producing a fluorinated organic compound that facilitates removal or separation of an auxiliary agent and that is advantageous in terms of production costs. The production method is a method for producing a difluoride which is a compound represented by formula (1) (in the formula, R1, R2, and n have the same definitions as the symbols described in the specification). The method involves a step for reacting the compound represented by formula (1) with (A) at least one fluorine source selected from hydrogen fluoride, hydrogen fluoride salts, and fluoride salts, (B) at least one iodine source selected from iodine and ammonium iodide, and (C) a compound having at least one fluorinated quaternary nitrogen atom in the molecule to difluorinate the compound represented by formula (1), wherein the amount of the iodine source (B) used is less than 1.0 mol with respect to 1 mol of the compound represented by formula (1).

The chlorination reaction kettle comprises a kettle body, the distributor assembly is arranged in the kettle body, the distributor assembly is composed of two distributors, the distributor located on the lower portion of the kettle body is connected with a hydrogen chloride inlet pipe, a spray head is installed above the distributor located on the upper portion of the kettle body, and the spray head is connected with the hydrogen chloride inlet pipe. A jacket is arranged between the inner wall and the outer wall of the kettle body; a glycerol storage tank is mounted on the left side of the kettle body, a glycerol pump is arranged on the right side of the glycerol storage tank, a glycerol inlet pipe is connected between the glycerol storage tank and the glycerol pump, and a glycerol outlet pipe is connected between an outlet of the glycerol pump and the kettle body; a pressure relief pipe is connected between the kettle body and the pressure relief tank, and a pressure relief valve is mounted on the pressure relief pipe. According to the utility model, the problems in the prior art can be solved, and better economic benefits can be created.

The present disclosure relates to processes for the fluorination of molecules. One aspect provides a process for incorporating a fluorine atom into a molecule, said process comprising converting a compound of formula X-SG into a compound of formula X-F, wherein G is an optionally substituted C1-C6 alkyl group, an optionally substituted aryl group, or an optionally substituted heteroaryl group, and X is an organic group; and wherein the SG group is attached to a secondary or tertiary carbon atom in the organic group X; said process comprising treating said compound of formula X-SG with (i) an activator compound selected from the group consisting of N-halosuccinimides, N-halobenzenesulfonimides, N-halobenzenesulfonamides, dialkylaminodihalosulfinium salts, heterocyclylaminodihalosulfinium salts, dialkylaminosulfur trihalides, XeF2, difluoroiodotoluene, di- and tri-bromoisocyanuric acids, bromine, chlorine, hypervalent iodine compounds with I2; and other sources of Br+, Cl+, F+, I+, bromonium, iodonium, or chloronium; and (ii) a source of fluoride. Uses of the process in the preparation of various fluorinated molecules as well as uses of certain compounds as intermediates in the processes of the present disclosure are also provided.

The application belongs to the technical field of chemical industry, and particularly relates to a sulfated titanium-iron oxide, a preparation method and application thereof. FeCl3 solution is added into an oxidized cellulose aqueous solution, and first mixing and stirring is carried out, then TiCl4 solution is added, second mixing and stirring is carried out, and then ammonia water is added drop by drop into the mixed solution to adjust the pH value to 8.6-9.2; a precipitate is obtained, the precipitate is filtered and washed, and then is immersed in a sulfuric acid solution, and then is fully washed and calcined to obtain the sulfated titanium-iron oxide. The catalyst provided by the application not only has high catalytic effect, but also maintains good catalytic activity and selectivity in the reaction process, and the catalyst can be recycled and reused through an external magnetic field.

To provide a method for preparing a partially fluorinated alcohol (fluorohydrin) from a fluorinated epoxide, and a method for preparing a fluorinated carbonate from a fluorohydrin.SOLUTION: Methods for preparing partially fluorinated alcohols (fluorohydrins) include, for example, preparing a fluorohydrin by reacting a fluorinated epoxide with a fluorinating agent (Olah's reagent) to effect ring opening, as in the following equation: Further, by reacting the obtained fluorohydrin with phosgene, it is possible to prepare the corresponding carbonic acid ester.SELECTED DRAWING: None

The present invention discloses novel method for synthesizing vegan 25-OH cholesterol / Calcifediol from inexpensive crude phytosterol. According to the method, Phytosterols are reacted to form corresponding i-steroid through tosylation and methanolysis. i-steroid on reductive ozonolysis to C-22 alcohol and conversion via C-22 tosylate to C-22 iodide in good yield. Coupling of C-22 tosylate with Grignard reagent of 4-bromo-2-methyl-2-[(trimethylsilyl)oxy] butane followed by deprotection yielded 25-OH cholesterol. In a process variant, nickel mediated conjugate addition of C-22 iodide to an electron deficient alkene ethyl acrylate and treating corresponding ester with methyl magnesium bromide as means of installing the side chain of 25-OH cholesterol in high yield. Further bromination reaction of 25-OH cholesterol diacetate followed by dehydrobromination using TBAF yielded 25-OH 7-dehydrocholesterol. Further photo reaction of 25-OH 7-dehydrocholesterol in to previtamin D3 using high or medium pressure mercury lamp and subsequent thermal reaction of previtamin D3 to 25-OH vitamin D3(Calcifediol) in good yield.

The application discloses a method for continuously synthesizing cis-13-octadecenal based on a micro-channel reactor, and belongs to organic synthesis. The method comprises unilateral bromination, acetylene coupling, selective hydrogenation, oxidation and purification. The method uses dodecanediol and 1-hexyne as raw materials, forms a method for continuously synthesizing cis-13-octadecenal, a key component of insect sex pheromone, in a high-efficiency and high-selectivity manner by using a micro-channel reactor, and effectively solves the problems of low cis selectivity, poor reaction efficiency and incapability of amplification effect in the synthesis of cis-13-octadecenal in the prior art.

The present disclosure includes brominated alkenyl alcohols, their use as flame retardants in polyurethanes and polyurethane foams, and polyurethanes containing brominated alkenyl alcohols. The present disclosure also provides compositions, methods, and processes. Brominated alkenyl alcohols used as flame retardants in polyurethanes can be generally described by Formula I, the scope of which is disclosed herein. [Formula 1] TIFF2022517533000023.tif44165

This invention provides a method for improving the utilization rate of hydrogen chloride in the chlorination reaction of glycerol, comprising the following steps: (1) passing the chlorinated distillate, the reactive distillation kettle liquid, and the light component and a portion of the heavy component material from the separation unit into a prechlorination reaction unit for prechlorination reaction to obtain gaseous material and prechlorinated reaction liquid; (2) passing glycerol containing a catalyst and the gaseous material into a reactive distillation unit for mixing reaction to obtain aqueous material and reactive distillation kettle liquid; (3) passing hydrogen chloride and the prechlorinated reaction liquid into a chlorination reaction unit for chlorination reaction to obtain chlorinated distillate and chlorinated liquid from the bottom of the tower; (4) passing the chlorinated liquid from the bottom of the tower into a separation unit to obtain dichloropropanol, light component, and heavy component material. The method provided by this invention efficiently utilizes the hydrogen chloride in the chlorinated gaseous material, improves the utilization rate of hydrogen chloride in the chlorination reaction of glycerol, and reduces alkali consumption and energy consumption, thereby achieving stable and clean production of epichlorohydrin using the glycerol method.

To provide a new method for producing a fluorinated organic compound in which removal or separation of an auxiliary is easy and which is advantageous in production cost.SOLUTION: A compound represented by the following formula (1): wherein R1, R2 and n are as defined in the description. The method comprises reacting the compound represented by the formula (1) with (A) at least one fluorine source selected from hydrogen fluoride, a hydrogen fluoride salt and a fluoride salt, (B) at least one iodine source selected from iodine and ammonium iodide, and (C) a compound having at least one fluorinated quaternary nitrogen atom in the molecule. A step of difluorinating the compound represented by the formula (1), wherein the amount of the iodine source (B) used is less than 1.0 mol per 1 mol of the compound represented by the formula (1).SELECTED DRAWING: None

The application discloses a kind of organic synthesis technical field[ 18 F] radioactive labeling method of trifluoromethyl terminal olefin, under room temperature condition, using 3,3-difluoro allyl sulfonium salt as precursor, 18 F] KF / K222 or[ 18 F] TBAF as fluorination reagent, acetonitrile as solvent, can obtain very high radiochemical yield within 30 seconds, and functional group tolerance is excellent, specific reaction formula is as follows: the method provides a simple and efficient way for producing[ 18 F] trifluoromethylated terminal olefin compound, so that it can be applied to positron emission tomography imaging.The method for constructing 3,3-difluoro allyl sulfonium salt compound is easy to obtain raw materials, low cost, simple operation, safe and controllable, and the obtained product has high radioactivity yield.

The invention provides a catalyst for preparing dichloropropanol through glycerol chlorination as well as a preparation method and application of the catalyst, and belongs to the technical field of catalyst preparation. The catalyst comprises tin composite salt and a carboxyl functionalized molecular sieve; the tin composite salt is composed of tin salt and copper salt; the tin composite salt accounts for 2-15% of the total amount of the catalyst. The catalyst provided by the invention has the advantages of high catalytic efficiency, long-term high activity, high target product selectivity, adjustable acidity, easy separation from the product, and no corrosion to equipment.

The invention provides a preparation method and a production system for preparing dichloropropanol through glycerol chlorination, and belongs to the technical field of compound preparation. According to the method, multi-stage series reaction kettles are adopted for reaction, and the chlorination reaction process is precisely regulated and controlled by controlling the reaction temperature and the dehydration amount. In the reaction, hydrogen chloride gas is communicated with all stages of reactors, glycerol and a catalyst are introduced into a first-stage reaction kettle for reaction, a liquid-phase product is transferred into a next-stage reaction kettle for continuous reaction, and a gas-phase product is dehydrated and then transferred into an original reaction kettle for continuous reaction. The method provided by the invention not only can accurately and efficiently solve the problem of moisture inhibition in the reaction process, but also can improve the chlorination reaction efficiency and the selectivity and yield of dichloropropanol, and improve the purity of the product.