71results about "Preparation by halogen introduction" patented technology

Provided is an organic photocatalyst that includes a compound represented by formula (1). The organic photocatalyst can use visible light from a blue LED or the like as a light source, has excellent stability under photoirradiation, can be recycled without losing catalytic activity, and can be used for large-scale synthesis. (In formula (1), R1–R11 are each independently a hydrogen atom, an alkyl group, an aryl group, an alkoxy group, an aryloxy group, an amino group, a heterocyclic aromatic group, or a halogen atom (excluding R1, R6, and R9 being a hydrogen atom), R1 and R2, R2 and R3, R3 and R4, R4 and R5, R5 and R6, R6 and R7, R8 and R9, or R9 and R10 may form a ring structure, X is a nitrogen atom or a boron atom, and Y and Z are each independently a sulfur atom, an oxygen atom or -NR12- (R12 being an alkyl group or an aryl group).)

A compound represented by the following formula (1):wherein RG is a group containing at least one cyclic structure,I is an iodine atom,R1 is a monovalent functional group having 0 to 30 carbon atoms, containing no polymerizable unsaturated bond, and being optionally the same or different;n is an integer of 1 to 5, andm is an integer of 1 to 5.

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.

The invention discloses a method for preparing ditrimethylolpropane, which comprises the following steps: a) trimethylolpropane and a brominating reagent are subjected to nucleophilic substitution reaction under the action of a catalyst I to obtain 2-bromo-2-ethyl-1, 3-propylene glycol; b) generating 2, 2-dimethylolbutanol sodium from trimethylolpropane under the action of a catalyst II; and c) carrying out a reaction on the 2, 2-dimethylol sodium butoxide and 2-bromo-2-ethyl-1, 3-propylene glycol under the action of a catalyst III to obtain the ditrimethylolpropane. The method has the advantages of high yield, few byproducts and high purity.

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.

Ortho-phthaldehyde is introduced as a versatile moiety to imbue ultraviolet-absorbing or visible chromophore compounds bearing this moiety with the capability to remain locally retained in the epidermis for days to weeks by virtue of a safe, efficient, and reagent-free reaction that bonds the ortho-phthalaldehyde moiety covalently to endogenous proteins in the stratum corneum of skin tissue by forming a phthalimidine linkage with primary aliphatic amines such as lysine and N-terminal residues, when applied topically on human or other mammalian skin from a suitable liquid, gel, or emulsion containing the ortho-phthalaldehyde compound with cosmetically acceptable alcohols, oils, and modifiers.

The invention discloses a preparation method of 3-bromo-1-propanol, comprising the following steps: preparing hydrobromic acid aqueous solution in a batching kettle; 1,3-propylene glycol and toluene are respectively delivered to a continuous batching kettle with a metering pump to mix and obtain a mixed solution A; the preheating temperature range of a microchannel reactor is controlled, the flow rate of the hydrobromic acid aqueous solution and the mixed solution A is adjusted, and the reaction solution is pumped into the microchannel reactor respectively; after the reaction material flows out of the microchannel reactor, 3-bromo-1-propanol is obtained by post-processing. The preparation method of the present invention significantly shortens the reaction time, has good reaction temperature control, few by-products, high yield, high selectivity, and is more beneficial to industrialized amplification production.

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.

The present invention provides a method for producing an organic halogen compound, with which it is possible to produce an organic halogen compound with high selectivity and high yield. Disclosed is a method for producing an organic halogen compound, the method including a halogenation step for halogenating a compound represented by formula (1α), which is a starting material, to obtain an organic halogen compound A represented by formula (1). In the halogenation step, halogenation is carried out in a multiphase system which includes an organic phase that contains an organic solvent as a solvent and an aqueous phase that contains water as a solvent.

The invention relates to the technical field of fine chemical engineering, and particularly discloses a preparation method and a catalyst of 2-chloroethanol. Activated carbon provided by the invention has a high specific surface area and a porous structure, can be used as a mass transfer channel to promote diffusion of ethylene glycol and HCl to ZrO2 active sites, and can be used for preparing 2-chloroethanol through an addition reaction between double bonds. Maleic acid is grafted on the composite carrier, a carboxylic acid group passes through hydroxyl of protonated ethylene glycol to form a protonated intermediate, the nucleophilicity of the hydroxyl is reduced in the process, the electron deficiency of hydroxyl oxygen is enhanced, the hydroxyl oxygen is more easily substituted by Cl <->, and the catalytic effect of the catalyst is improved under the combined action of the carboxylic acid group and zirconium oxide; meanwhile, the activated carbon serves as a solid supporting body, so that the catalyst is easily recycled through filtration or centrifugation, the problem that a traditional homogeneous catalyst (such as adipic acid) is difficult to recycle is solved, and in addition, the catalyst provided by the invention still has a good catalytic effect after being recycled and reused.

The invention belongs to the technical field of synthesis, and particularly relates to a small reactor for preparing a chilo suppressalis pheromone intermediate and application of the small reactor. According to the small reactor, rapid mixing is achieved through a threaded mixing pipe, the introduction amount of a hydrobromic acid solution is controlled in the mixing process, and a reaction from low concentration to unilateral bromination of hydrobromic acid is achieved; meanwhile, a mixed solution obtained after the bromination reaction is mixed with a sodium bicarbonate solution in a spraying mode, the washing neutralization effect is achieved, standing, cooling and layering are formed through pressure release valves arranged in a gradient mode, and finally a methylbenzene solution and an aqueous solution are obtained. The method is mild in reaction condition, short in reaction time, high in reaction efficiency, high in automation degree, low in energy consumption and good in safety, meets the green chemical engineering concept and is easy to industrially apply.

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.

Disclosed herein are processes for preparing certain intermediates useful in the synthesis of 3-fluoro-5-(((1S,2aR)-1,3,3,4,4-pentafluoro-2a-hydroxy-2,2a,3,4-tetrahydro-1H-cyclopenta[cd]inden-7-yl)oxy)benzonitrile or a pharmaceutically acceptable salt thereof.

The utility model relates to the technical field of dichloropropanol preparation through chlorination, in particular to a production device for preparing dichloropropanol through glycerol tower type chlorination. Comprising a first-stage reaction unit and a second-stage reaction unit, the first-stage reaction unit comprises a first-stage chlorination tower, a first-stage circulation kettle connected to the first-stage chlorination tower and a first-stage circulation heat exchanger connected between the first-stage chlorination tower and the first-stage circulation kettle, and a first-stage chlorination tower condenser is arranged at the top of the first-stage chlorination tower; the second-stage reaction unit comprises a second-stage chlorination tower, a second-stage circulation kettle connected to the second-stage chlorination tower, and a second-stage circulation heat exchanger connected between the second-stage chlorination tower and the second-stage circulation kettle; a second-stage chlorination tower condenser is arranged at the top of the second-stage chlorination tower; according to the utility model, a gas-phase material and a liquid-phase material can be mixed more uniformly, moisture can be efficiently and timely moved out of a reaction system, the positive reaction rate is high, the conversion rate of glycerol and hydrogen chloride is high, and the energy consumption is reduced.

The present invention refers to a process for the functionalization such as a deaminative halogenation of an aromatic or heteroaromatic amino compound. With the inventive process, the in-situ nitrate reduction allows the direct ipso-halogenation of anilines and aminoheterocycles via an aryldiazonium or heteroaryl diazonium salt as a fleeting intermediate in solution.

The invention belongs to the technical field of synthesis of organic chemicals, and particularly relates to a synthesis method of 3-fluoro-1-propanol. The synthesis method of the 3-fluoro-1-propanol comprises the following steps: mixing 3-chloro-1-propanol with fluoride, a catalyst and an organic solvent, carrying out a heating reaction under a stirring condition, monitoring the consumption of raw materials and the generation condition of a product, ending the reaction until the selectivity of the product is not improved any more, continuously stirring the obtained reaction liquid, and cooling to room temperature to obtain the 3-fluoro-1-propanol. And adding water which is 1-2 times of the volume of the reaction liquid, extracting by adopting an extracting agent, removing water from an organic phase, carrying out reduced pressure distillation, and collecting fractions to obtain the 3-fluoro-1-propanol. The molar ratio of the 3-chloro-1-propanol to the fluoride is 1: (1.2-1.5). The fluoride is one of potassium fluoride, sodium fluoride, cesium fluoride or tetrabutylammonium fluoride. The synthesis method of 3-fluoro-1-propanol provided by the invention has the advantages of mild reaction conditions, high selectivity, low cost and environmental friendliness.

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.

This invention provides polyurethane foams containing a brominated flame retardant. Also provided are formulations and methods for preparing polyurethane foams containing a brominated flame retardant.

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+, l+, 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 invention discloses a device and a method for preparing dichloropropanol through a microchannel chlorination reaction, and relates to the technical field of dichloropropanol. Comprising a bottom plate, mounting bases are mounted on the two sides of the outer wall of the top of the bottom plate, a main pipe is mounted on the inner walls of the tops of the mounting bases, and air pressure adjusting mechanisms are mounted in and above the main pipe. The reaction bin is arranged to provide a space for reaction of chlorine and propylene, the pressure in the reaction bin can be adjusted through the air pressure adjusting mechanism, and the temperature in the reaction bin can be adjusted through the temperature control mechanism. The internal environment of the reaction bin is adjusted to be suitable for the reaction of chlorine and propylene according to the combination of the actual environment and the suitable environment, so that the efficiency of the chlorination reaction is improved, heat released during the chlorination reaction can be counteracted by adjusting the temperature, and the influence of heat accumulation on the reaction bin and reaction products is reduced; the chlorine and the propylene can be fully mixed, so that the reaction efficiency is improved.

Provided is a novel method for producing a fluorinated organic compound. This production method is a method for producing a fluorine adduct of a compound represented by formula (1) # imgabs0 # (in the formula, R1, R2 and n are as defined in the symbols described in the description. ) The production method comprises: a step for reacting a compound represented by formula (1) with (A), (B), and (C), and adding fluorine to the double bond or triple bond: (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, an iodo-aliphatic compound and an iodo-aromatic ring compound; and (C) at least one compound selected from the group consisting of compounds represented by formula (2-1) having or not having one or more substituents, and multimers thereof: # imgabs1 # (in the formula, X represents a conjugated base of a Bronsted acid. ).

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.

The present invention belongs to the technical field of the synthesis of organic chemicals, and particularly relates to a method for synthesizing 3-fluoro-1-propanol. The method for synthesizing 3-fluoro-1-propanol according to the present invention: mixing 3-chloro-1-propanol with a fluoride, a catalyst and an organic solvent, and carrying out a heating reaction under stirring conditions, monitoring the consumption of raw materials and the formation of products, and ending the reaction until the product selectivity no longer increases. For the obtained reaction solution, continuously stir and cool it to room temperature, add water in an amount 1-2 times the volume of the reaction solution, extract with an extractant, dehydrate the organic phase, distill under reduced pressure, collect the fractions, and obtain 3-fluoro-1-propanol. The molar ratio of the 3-chloro-1-propanol to the fluoride is 1:1.2-1.5. The fluoride is one of potassium fluoride, sodium fluoride, cesium fluoride or tetrabutylammonium fluoride. The method for synthesizing 3-fluoro-1-propanol provided by the present invention has mild reaction conditions, high selectivity, low cost, and is environmentally friendly.

The invention provides a production process for co-production of 3-chloropropene and dichloropropanol and a device and application thereof, the production process comprises the following steps: raw materials propylene and chlorine are subjected to a halogenation reaction in a halogenation reactor, a halogenation reaction product enters a heat exchanger to be subjected to heat exchange and then is divided into a gas phase part and a liquid phase part, the hydrogen chloride gas in the gas phase part is used as a raw material and is subjected to a hydrochlorination reaction with glycerol and a catalyst in a hydrochlorination reactor for preparing dichloropropanol; according to the method, a large amount of hydrogen chloride as a byproduct in the propylene high-temperature chlorination process is fully utilized and supplied to a chlorine source required in the glycerol hydrochlorination process, so that the byproduct recovery treatment process in the propylene high-temperature chlorination process is omitted, the production process is simplified, the energy consumption is reduced, and the device is simple to operate, low in cost and high in yield. The equipment is high in production efficiency and beneficial to industrial application.

The invention relates to the field of chemical production processes, in particular to a method for preparing dichloropropanol through glycerol chlorination. The invention relates to a method for preparing dichloropropanol by glycerol chlorination, which comprises the following steps: adding a catalyst into an adipic dialdehyde solution, introducing crude hydrogen chloride gas, and filtering after reaction to obtain feed liquid and hydrogen chloride gas; cooling the feed liquid, filtering and drying to obtain adipic acid crystals and a hydrochloric acid solution; and dissolving the adipic acid crystal in preheated glycerol, introducing hydrogen chloride gas, and reacting to obtain dichloropropanol. According to the present invention, the oxidation reduction reaction is performed on the adipaldehyde and the chlorine gas in the crude hydrogen chloride gas under the action of the catalyst, such that the chlorine gas impurity is effectively absorbed so as to reduce the probability of the side reaction of the chlorine gas and the glycerol so as to significantly improve the yield of the dichloropropanol; meanwhile, adipic acid generated by the reaction can be used as a catalyst for subsequent preparation of dichloropropanol from glycerol and hydrogen chloride gas, and a generated hydrochloric acid solution can be recycled and used for dissolving adipic dialdehyde, so that efficient utilization of resources is realized.

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).