333results about "Preparation by halogen introduction" patented technology

The invention relates to fused cyclooctyne compounds, and to a method for their preparation. The invention also relates to a conjugate wherein a fused cyclooctyne compound according to the invention is conjugated to a label, and to the use of these conjugates in bioorthogonal labeling, imaging and/or modification, such as for example surface modification, of a target molecule. The invention further relates to a method for the modification of a target molecule, wherein a conjugate according to the invention is reacted with a compound comprising a 1,3-dipole or a 1,3-(hetero)diene.

The present invention relates to a process for converting a multihydroxylated-aliphatic hydrocarbon or ester thereof to a chlorohydrin, by contacting the multihydroxylated-aliphatic hydrocarbon or ester thereof starting material with a source of hydrogen chloride at superatmospheric, atmospheric and subatmospheric pressure conditions for a sufficient time and at a sufficient temperature, preferably wherein such contracting step is carried out without substantial removal of water, to produce the desired chlorohydrin product; wherein the desired product or products can be made in high yield without substantial formation of undesired overchlorinated byproducts; said process carried out without a step undertaken to specifically remove volatile chlorinated hydrocarbon by-products or chloroacetone, wherein the combined concentration of volatile chlorinated hydrocarbon by-products and chloroacetone is less than 2000 ppm throughout any stage of the said process.

The present invention relates to a process for converting a multihydroxylated-aliphatic hydrocarbon or ester thereof to a chlorohydrin, by contacting the multihydroxylated-aliphatic hydrocarbon or ester thereof starting material with a source of a superatmospheric partial pressure of hydrogen chloride for a sufficient time and at a sufficient temperature, and wherein such contracting step is carried out without substantial removal of water, to produce the desired chlorohydrin product; wherein the desired product or products can be made in high yield without substantial formation of undesired overchlorinated byproducts. In addition, certain catalysts of the present invention may be used in the present process at superatmospheric, atmospheric and subatmospheric pressure conditions with improved results.

A method of preparing for dichloropropanol from glycerol is that the glycerol and catalyst are added into a spraying type reactor; a liquid circulating pump is used to pump the glycerol and the catalyst our from the spraying type reactor, then the glycerol and the catalyst are sent into the spraying type reactor from the top of the spraying type reactor by the manner of spraying; HCl gas which is absorbed from the lateral part of the spraying type reactor is mixed completely and react with the materials of the glycerol and the catalyst inside the spraying type reactor; at the same time the negative pressure produced by spraying brings a resultant inside the spraying type reactor in the form of an azeotropic matter of water, the dichloropropanol and the HCl; the water and the dichloropropanol in the azeotropic matter are condensed down by a condenser, and the unreacted HCl gas and the complementary HCl gas are sent into the spraying type reactor together for cyclic reaction. The invention has the advantages of the improvement of the reaction velocity and high glycerol transformation rate.

The present invention relates to a process for the production of dichlorohydrin by catalyzed hydrochlorination of glycerine where the reaction is performed in at least two subsequent stages operating continuously at different pressures with both vapor and liquid recycle. The first reactor, low pressure (L. P.) reactor, operating at a pressure ranging from 1 to 4 bar and at a temperature from 900C to 1300C converts most of GLY to MHC. The second reactor, medium pressure (M. P. ) reactor, operating at a pressure ranging from 5 to 20 bar and at temperature from 90 DEG c to 1300C converts the effluent from the L. P. reactor to DCH with an adequate degree of conversion. Each reactor is followed by a stripping unit.

The invention discloses a technique for preparing dichloropropanol by the autocatalytic reaction of glycerol and hydrogen chloride. Glycerol and hydrogen chloride carry out autocatalytic reaction at the temperature of 105 to 160 DEG C and the pressure of 0.05 to 0.5Mpa, and the water generated in the reaction is distilled and removed. The invention also discloses a system for preparing dichloropropanol by the autocatalytic reaction of glycerol and hydrogen chloride gas. By adopting the technique of autocatalytic reaction of glycerol and hydrogen chloride, the invention avoids the using of catalyst, lowers production cost obviously, eliminates the formation of by-products with high boiling point, improves reaction selectivity and has the advantages of simple technique and low production cost. The system can transform glycerol fully and greatly improves the selectivity of dichloropropanol; the purity of the dichloropropanol obtained finally is more than 99.5 percent.

The invention relates to a production method of dichloropropanol, comprising the following reaction steps: glycerol reacts with gaseous HCl in the presence of organic carboxylic acid catalyst, reaction liquid reactant reacts with gaseous HCl in the presence of Lewis acid catalyst and then reacts with gaseous HCl again under the action of microwave and the stirring action; after passing through a low-boiling-point substance distillation tower and a rectifying tower, the mixture is prepared into the product of the invention. Compared with the prior art, HCl conversion rate is improved by about one time. When the combined catalysis technology of the invention is adopted, the dosage of the organic carboxylic acid catalyst is lowered by half, glycerol conversion rate is improved by 2%, and product yield is improved by 5%; and meanwhile, side reaction is reduced so as to avoid the defect that extra potentially toxic organic carboxylic acid side reaction generates a great quantity of waste, thus protecting environment.

The invention relates to a decarboxylation and fluorination method of vinyl carboxylic acid. In the method, in an aqueous or polar organic solvent or a mixed solvent of aqueous and polar organic solvents, vinyl carboxylic acid, an additive and an electrophilic fluorinating reagent are reacted at room temperature-reflux temperature so as to synthesize monofluoro olefin, allyl fluoride, difluoro alkyl substituted alcohol, mono-difluoro alkyl substituted alcohol, monofluoro alkyl substituted epoxide, beta-monofluoro/difluoro substituted cyclic lactone or beta-monofluoro substituted unsaturated cyclic lactone compounds. The structural formula of vinyl carboxylic acid is shown in the specification. According to the method in the invention, raw materials are available, reaction is simple and convenient, and the method can be used for preparing compounds which are difficult to prepare by using a common method.

The invention provides a production process for preparing dichloropropanol by reactive distillation of glycerol. The production process comprises the following steps: the raw material glycerol containing a homogeneous catalyst is sent to a reactive rectification tower from the top after heat exchange, hydrogen chloride gas enters from the lower part of a rectification section of the tubular reactive rectification tower, and the raw material glycerol and countercurrent flow of the hydrogen chloride gas are subject to absorption and chlorination reaction by a packing layer at the temperature of 90-120 DEG C and the temperature of 0.001-0.1MPa (absolute pressure) and are rectified; omonochloropropylene glycol at the bottom of the tubular reactive rectification tower, glycerol and glycerol oligomer are sent to a heavy constituent separation tower for decompressing and recovering the monochloropropylene glycol and the glycerol is returned to the raw material glycerol; and product gas on the top of tubular reactive rectification tower is cooled by a heat exchanger to obtain the dichloropropanol which is sent to a cyclization working procedure, and tail gas is further washed with lye, and is discharged from by a vacuum pump.

The object of the invention is to provide a method for synthesizing dichloropropanol with glycerin and hydrochloric acid. After pretreated industrial hydrochloric acid or pretreated industrial by-product hydrochloric acid or reagent hydrochloric acid is mixed with glycerin and catalyst in a batching tank, continuous Put it into a reactor equipped with a fractionation device on the top, continue heating under normal pressure for chlorination reaction, the temperature is controlled at 100-200°C, while continuously performing chlorination reaction, continuously distill the material in the reactor, and the product dichloro Propanol and water are continuously taken out from the reaction system after being condensed into liquid by the condenser; the same pretreatment method of industrial hydrochloric acid and industrial by-product hydrochloric acid of the present invention is to add one or more phosphorus-containing and/or sulfur-containing hydrochloric acid to the hydrochloric acid to be treated. Alkali metal and/or alkaline earth metal salts of inorganic acids, added in an amount of 0.1 to 15% of the weight of the hydrochloric acid to be treated, stirred at a temperature of 0 to 100°C for 0.5 to 15 hours; And the by-product hydrochloric acid provides a good outlet, which is conducive to reducing the production cost of dichloropropanol.

The invention relates to a method for preparing tranexamic acid. The method comprises the following steps: reacting 1,4-cyclohexanedimethanol, used as starting material, with an HX acid to generate 4-chloromethylcyclohexylmethanol or 4-iodomethylcyclohexylmethanol, carrying out an oxidation reaction in an atmosphere of a gas containing 21-100% of oxygen in order to produce 4-chloromethylcyclohexylcarboxylic acid or 4-iodomethylcyclohexylcarboxylic acid, carrying out an aminolysis reaction in an autoclave, introducing liquid ammonia or ammonia water having an ammonia content of 15-28% to the aminolysis reaction system, and transforming the obtained reaction product with an alkali after the aminolysis reaction is finished in order to obtain the tranexamic acid, wherein X is Cl or I. Comparedwith the prior art, the preparation method has the advantages of cheap and easily available raw materials and low cost. The method also has the advantages of simplicity in operation, high yield, andsuitableness for industrial production.

The invention relates to a method for synthesizing dichloropropanol by catalyzing glycerol for chlorination under the existence of dicarboxylic acid-rare earth chloride, which comprises the following steps of: mixing glycerol and a dicarboxylic acid-rare earth chloride composite catalyst in a chloridizing reactor R-1, and then introducing chlorine hydride gas, constantly evaporating out water and partial dichloropropanol generated in the reactor; introducing chlorine hydride as a tail gas into a chloridizing reactor R-2 filled with the glycerol and the catalyst; after the chlorination of the reactor R-1 is ended, evaporating dichloropropanol by decompression and then adding the glycerol for further chlorination; during the distillation of the chloridizing reactor R-1, starting to introduce chlorine hydride into the chloridizing reactor R-2, and the chlorine hydride as the tail gas into a chloridizing reactor R-3, wherein the glycerol and the catalyst added into the chloridizing reactors R-1, R-2 and R-3 have the same dosage; after the chlorination of the chloridizing reactor R-2 is ended, repeating the procedures of distillation, feeding and chlorination in the chloridizing reactor R-1; connecting the chloridizing reactors R-1,R-2 and R-3 from head to tail, and introducing the chlorine hydride as the tail gas into the chloridizing reactor R-1 while introducing the chlorine hydride into the chloridizing reactor R-3; transferring a mixed liquor of the dichloropropanol, water and the chlorine hydride to a distillation still, and adding an organic solvent to remove water by azeotropy. The method has the advantages of high reaction speed, high utilization ratio of the chlorine hydride and high yield.

The invention relates to improvement on a method for preparing dichlorohydrin by chlorinating glycerin and a reaction device. The chlorinating reaction is the series reaction of a reaction kettle and a sprinkling reaction tower which is filled with filler. The sprinkling reaction tower is sequentially provided with a placing filter zone, a hollow built-in sprinkling device zone and a placing filter zone from top to bottom. After viscosity decrease by kettle type preaction, the sprinkling reaction is carried out, the reaction contact is sufficient, the reaction time is long, the reaction efficiency is greatly enhanced, the conversion rate of the glycerin achieves 100%, and the reaction time is short and only needs 6-8 hours. The dichlorohydrin yield can be enhanced to more than 96%, and the yield can be enhanced to more than 99.0% by adding kreatine and strong acid mixing catalyst. The invention has the advantages of simple process flow, convenient reaction operation and high reaction efficiency.

A process for converting multihydroxylated-aliphatic hydrocarbon compound(s) and/or ester(s) thereof to chlorohydrins and/or esters thereof is disclosed in which one or more of multihydroxylated-aliphatic hydrocarbon compound(s) and/or ester(s) thereof and/or monochlorohydrin(s) and/or ester(s) thereof with at least one chlorinating feed stream comprising at least one chlorinating agent and at least one impurity having a boiling point below the boiling point of the chlorohydrin product having the lowest boiling under hydrochlorination conditions, optionally in the presence of water, one or more catalyst(s), and/or one or more heavy byproduct(s) in a reaction vessel under hydrochlorination conditions, wherein the liquid-phase reaction mixture is maintained at a temperature below the boiling point of the chlorohydrin product having the lowest boiling point under hydrochlorination conditions and greater than the boiling point(s) of the at least one impurity and a vapor phase vent stream comprising the at least one impurity is removed from the liquid phase reaction mixture. An apparatus suitable for carrying out the disclosed process is illustrated in FIG. 1 of the drawings. The process and apparatus improve conversion rates and/or provide for recovery of chlorinating agent for lower operating costs.

The invention provides a method for synthesizing dichloropropanol by glycerine, which comprises the following steps: the glycerine and organic acid are processed through esterification reaction under the catalysis of solid acid functioning as catalyst to generate organic acid glycerine ester, chlorine hydride is guided to the organic acid glycerine ester for chlorination reaction, and the dichloropropanol as the product of reaction is collected after the chlorination reaction finishes. The method for synthesizing dichloropropanol by glycerine is characterized in that firstly, during the esterification reaction of the glycerine and the organic acid under the catalysis of the solid acid, generated water is removed, thus the dissolution of the chlorine hydride during the esterification reaction is lessened, and the corrosion to equipment is reduced; secondly, high chlorination activity and rapid reaction speed are guaranteed through the esterification reaction, and particularly, the reaction time is markedly shortened under pressure; and thirdly, the dosage of the chlorine hydride is reduced and the environmental pollution is alleviated.

The invention provides a method for preparing dichloropropanol from glycerol through hydrochlorination, which comprises the steps as follows: (1) the mixing raw material liquid of activator and the glycerol is poured into an absorption reaction tower from the top thereof, hydrogen chloride is put into the absorption reaction tower from the bottom thereof, the materials at the bottom of the absorption reaction tower are partially sent back to the absorption reaction tower and parts are put into the first stirring vessel of n stirring vessels; (2) the hydrogen chloride is let into the first stirring vessel for carrying out reaction and then reaction solution enters into the second stirring vessel of the n stirring vessels to react with the hydrogen chloride, and the reaction solution reacts with the hydrogen chloride in the n stirring vessels in turn according to the process; (3) the condensate of the gaseous phase mixtures braised out from the tops of the stirring vessels are gaseous phase products and the mother liquor comes out from the nth stirring vessel is aqueous phase product. The method of the invention is low in investment on equipment, simple in operation and control and high in reaction speed, thus being easy for expanding production with the yield of dichloropropanol per pass higher than 90 percent and the use ratio of the hydrogen chloride higher than 70 percent.

The invention provides a method for using by-product glycerin of recyclable material bio-diesel as material to produce organic compounds as dichlorohydrin and epichlorohydrin. In the presence of catalyst carboxyl acid or relative derivative, glycerin is reacted with chlorizating agent as hydrochloride or alcaine to produce dichlorohydrin, and the dichlorohydrin in the presence of alkali is dewatered to produce epichlorohydrin.

The invention relates to a method for synthesizing a 1,3-diphenyl-1-propanol compound, belonging to a method for synthesizing a compound. P-substituted 1-phenyl ethanol and p-substituted benzyl alcohol are used as raw materials, wherein R and R' are hydrogen atoms, halogen atoms Cl, Br, alkyl and alkoxy, and the adding ratio of the substituted 1-phenyl ethanol to the substituted benzyl alcohol is1: (1-2). The method comprises the following steps of: sequentially adding a dry catalyst, alkali, substituted1-phenyl ethanol and substituted benzyl alcohol into an anhydrous solvent under the condition of nitrogen, placing a reactor into an oil bath of 125 to 135 DEG C, and stirring for 8 to 24 hours; cooling, neutralizing the reaction solution, performing extraction by using ethyl acetate, andconcentrating the extract in vacuum till no ethyl acetate smell; and performing chromatographic purification by using a positive silica gel column of 100 to 200 meshes. The invention has the advantages of simple, convenient and feasible method, low production cost, reduced difficulty of purification and post treatment and weakened influence on the environment.

The invention discloses a copper fluoride (I) reagent as well as a preparation method and an application thereof. The copper fluoride (I) reagent is prepared through the following steps: stirring cuprous chloride and sodium tert-butoxide in a tetrahydrofuran solvent at room temperature to react, and adding a nitrogen ligand and triethylamine trihydrofluoride so as to obtain the copper fluoride (I) reagent which is stable in air. The triethylamine trihydrofluoride serves as a fluorine element source of the reagent, and the reagent can efficiently catalyze haloalkane to form hydrofluoroalkane. The high-purity and high-yield copper fluoride (I) reagent can be directly obtained through utilizing the industrial low-cost cuprous chloride, and has good reactivity with the hydrofluoroalkane containing a plurality of important functional groups; and a metal fluorinated reagent can be prepared without using toxic compounds and precious metals, the cost and operation requirements can be greatly lowered, and the copper fluoride (I) reagent has a good industrial application prospect.

The invention belongs to the technical field of synthetic chemistry and particularly relates to a method for synthesizing 1-iodo-alkyne in a high-selectivity manner. The method is mild in reaction condition, controllable in reaction product, single in product, easy in product purification, high in chemical selectivity, simple in synthesizing step, safe, reliable, green, environmentally friendly, applicable to various terminal alkyne reaction substrates and suitable for industrial production, and the synthesizing yield of the method reaches up to 99%.

The invention discloses a method for preparing dichloropropanol with a chemical reaction-pervaporation coupling method, wherein the method provided by the invention comprises the following steps of: directly adding glycerol and a liquid catalyst into a chemical reactor (if a solid catalyst is used, putting the solid catalyst into the reactor in advance) after pre-heating, simutaneously feeding a hydrogen chloride gas into the reactor, chlorinating the glycerol with the hydrogen chloride in the reactor, instantly introducing the reaction product into a pervaporation device, wherein a permeable film in the device preferably permeates and removes water generated in the reaction to accelerate chlorination reaction efficiently, thereby finally obtaining the dichloropropanol with high concentration. The method provided by the invention couples the pervaporation device with the chemical reactor to instantly remove the water generated in the reaction, thereby improving the efficiency of the chlorination reaction, reducing the hot load in the subsequent dehydration process of a dichloropropanol rectifying column, and improving the utilization efficiency of hydrogen chloride.