- Synthesis method of substituted phenoxyacetate compound
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The invention discloses a synthesis method of a substituted phenoxyacetate compound, relates to a synthesis method of a compound and aims to solve the problems that during current preparation of the substituted phenoxyacetate compound by a condensation method, a large amount of organic agent is consumed, substituted phenol is unlikely to react completely, the content of free phenol in three wastesis high and a very high environmental risk exists. According to the synthesis method, after the substituted phenol is mixed with haloacetate, a condensation reaction is performed in a potassium fluoride system condensing agent under the synergistic catalysis of a phase transfer catalyst and a halogenated hydrocarbon activator to obtain a substituted phenoxyacetic acid compound. The synthesis method is applied to the field of compound synthesis.
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Paragraph 0065; 0066; 0067
(2019/08/01)
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: S1) carrying out 2-site and/or 4-site selective chlorinationreaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, the catalyst B has the following structural formula of R1'-S-R2', and the phenoxycarboxylic ester has any structure represented by the formulas I-IV; and S2) carrying out transesterification reaction of chlorophenoxycarboxylic ester and alcohol under the action of a catalyst to obtain long-chain chlorophenoxycarboxylic ester, wherein the alcohol has the molecular formula of R2OH, and R2 is C4-20 alkyl or cycloalkyl. The method improves the yield and purity of chlorophenoxycarboxylic ester by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content ofthe obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 98.5% or more.
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Paragraph 0071; 0073; 0075; 0077; 0078; 0080; 0099; 0101
(2019/01/08)
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: S1) carrying out 2-site and/or 4-site selective chlorinationreaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, the catalyst B is C5-22 thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof, and the phenoxycarboxylic ester has any structure represented by the formulas I-IV; and S2) carrying out transesterification reaction of chlorophenoxycarboxylic ester and alcohol under the action of a catalyst to obtain long-chain chlorophenoxycarboxylic ester, wherein the alcohol has the molecular formula ofR2OH, and R2 is C4-20 alkyl or cycloalkyl. The method improves the yield and purity of chlorophenoxycarboxylic ester by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content of the obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 98.5% or more.
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Paragraph 0088; 0090
(2019/01/08)
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- A phenoxy carboxylic acid ester herbicide preparation method (by machine translation)
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The invention provides a phenoxy carboxylic acid ester herbicide preparation method, including: S1, phenol in the presence of alkaline substance with the chlorinated carboxylic acid ester condensation reaction, phenoxy carboxylic acid ester obtained; the ClR states the chloro- carboxylic acid ester of the general formula1 COOR, R1 Is C1 - 3 alkylene or alkylidene, R is C1 - 10 alkyl or C3 - 10 cycloalkyl; S2, the [...] ester in the 1st and 2nd catalyst the presence of a catalyst, with the chlorinating agent to carry out the selective chlorination of, get [...] ester; the Lewis acid catalyst is selected from the 1st, the 2nd catalyst is C5 - 22 of the thioether, thiazole, thiophene compounds or different benzisothiazoles; S3, will the [...] ester with an alcohol reaction, as shown in formula I phenoxy carboxylic acid ester herbicide; R3 Is H, Cl or CH3 , R ' is a C4 - 20 alkyl or cycloalkyl. This invention can improve the product quality and the production environment, three waste low. (by machine translation)
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- Preparation method of 2,4-dichlorophenoxyacetic ester
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The invention provides a preparation method of 2,4-dichlorophenoxyacetic ester, wherein the preparation method includes the following steps: S1) carrying out a reaction of phenol and methyl chloroacetate under alkaline conditions to obtain methyl phenoxyacetate; S2) carrying out selective chlorination reaction of methyl phenoxyacetate with a chlorinating agent under the action of a catalyst A anda catalyst B to obtain 2,4-methyl dichlorophenoxyacetate, wherein the catalyst A is Lewis acid, and the catalyst B is C5-22 thioethers, thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof; and S3) carrying out transesterification reaction of 2,4-methyl dichlorophenoxyacetate and alcohol under the action of a catalyst, to obtain 2,4-dichlorophenoxyacetic ester, wherein the alcohol is C2-20 alcohol. The selective chlorination reaction is carried out with methyl phenoxyacetate as a raw material, the selectivity of the reaction is improved, the loss of effective components isavoided, the yield of the effective components is greatly improved, and the three-waste treatment capacity, the three-waste treatment difficulty and the treatment cost are reduced.
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: carrying out 2-site and/or 4-site selective chlorination reaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, and the catalyst B is C5-22 thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof. The method effectively improves the chlorination selectivity and avoids loss of effective ingredients by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content of the obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 99% or more.
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Paragraph 0061; 0062
(2019/01/06)
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: carrying out 2-site and/or 4-site selective chlorination reaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, and the catalyst B has the following structural formula of R1'-S-R2'. The method effectively improves the chlorination selectivity and avoids loss of effective ingredients by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content of the obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 99% or more.
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Paragraph 0072; 0073
(2019/01/08)
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- A [...] ester preparation method (by machine translation)
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The invention provides a method for preparing [...] ester, including: the phenoxy carboxylic acid ester compounds, supported Lewis acid catalyst, sulfur-containing polymer mixed with the chlorinating agent, the selective chlorination reaction, to obtain [...] ester. Compared with the prior art, this invention uses benzene oxygen suo acid ester compound as a raw material obtained by the selective chlorination of [...] ester, simple preparation method, to avoid having the bad smell of the Fe0 production and use, thereby fundamentally preventing the substance to the dioxin generation; at the same time supported Lewis acid and sulfur-containing polymer common as catalyst, through the two cooperative positioning function, the selectivity of the dichloride to improve, and the two can through the filter recovery and re-use, the use of the recycling of the catalyst; furthermore the invention avoids the losses of the active ingredient, the extraction rate of the product, reduces energy consumption, prevent high COD, the generation of high salt waste water, three waste output has been largely reduced. (by machine translation)
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Paragraph 0056; 0057
(2019/01/08)
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- Preparation method of 2,4-dichlorophenoxyacetic acid and salt thereof
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The invention provides a preparation method of 2,4-dichlorophenoxyacetic acid and a salt thereof, wherein the preparation method includes the following steps: S1) carrying out a reaction of phenol andchloracetic ester under alkaline conditions to obtain phenoxyacetic ester; S2) carrying out selective chlorination reaction of the phenoxyacetic ester with a chlorinating agent under the action of acatalyst A and a catalyst B to obtain 2,4-dichlorophenoxyacetic ester, wherein the catalyst A is Lewis acid, and the catalyst B is C5-22 thioethers, thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof; and S3) carrying out hydrolysis reaction of 2,4-dichlorophenoxyacetic ester under acidic conditions to obtain 2,4-dichlorophenoxyacetic acid; or after 2,4-dichlorophenoxyaceticester is obtained, carrying out an alkaline hydrolysis reaction with an alkaline compound to obtain 2,4-dichlorophenoxyacetate. The production and use of 2,4-dichlorophenol with unpleasant odor are avoided, the production of dioxins is eliminated, the yield of products is improved, and the output of three wastes is greatly reduced.
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Paragraph 0099; 0101
(2019/01/06)
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- Preparation method of phenoxycarboxylic acid choline salt
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The invention provides a preparation method of a phenoxycarboxylic acid choline salt, wherein the preparation method includes the steps: S1, carrying out condensation reaction of phenol or o-cresol with chlorocarboxylic ester in the presence of alkaline substances to obtain phenoxycarboxylic ester; S2, carrying out selective chlorination of the phenoxycarboxylic ester with a chlorinating agent inthe presence of a first catalyst and a second catalyst to obtain chlorobenzoxycarboxylic ester; and S3, after reaction of trimethylamine with ethylene oxide, adding the chlorophenoxycarboxylic acid ester, and carrying out alkaline hydrolysis reaction to obtain the phenoxycarboxylic acid choline salt. Compared with a conventional synthesis technology, the preparation method effectively avoids the production and use of chlorophenols with unpleasant odor, radically eliminates the production of highly toxic dioxins, and greatly improves the product quality and the operation environment of the production site; with phenol as the raw material, through condensation, selective chlorination and alkaline hydrolysis, the high-quality phenoxycarboxylic acid choline salt is obtained, the loss of effective ingredients is effectively avoided and the yield of the product is increased.
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Paragraph 0071; 0073
(2019/01/08)
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- A method for preparing 2, 4 - dichlorophenoxyacetic acid (by machine translation)
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The invention provides a 2, 4 - dichlorophenoxyacetic acid preparation method, comprising: A) a halogenated acetic acid with the monoester should be halogenated acetate; phenol with alkali reaction to obtain the phenoxide; B) halogenated acetate and phenol salt reaction to obtain the phenoxyacetic acid ester; C) phenoxyacetic acid ester under the effects of catalyst chloride to obtain 2, 4 - dichlorophenoxy ester; said catalyst selected from iron trichloride, aluminum trichloride, boron trifluoride, five [...], trifluoromethyl sulfonate, aluminum oxide, ferric oxide, boron trioxide, niobium pentoxide, diphenyl ether, diphenyl sulfide, benzoin two sulfide, dimethyl sulfide and dimethyl sulfide in one or several of the D) 2, 4 - dichlorophenoxy ester hydrolysis to obtain 2, 4 - dichloro acid. This invention adopts the specific reaction routes and chlorinated using a specific catalyst, good reaction selectivity, few by-products, high yield. (by machine translation)
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Paragraph 0053; 0054
(2018/09/08)
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- A method for preparing 2, 4 - dichlorophenoxyacetic acid (by machine translation)
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The invention provides a 2, 4 - dichlorophenoxyacetic acid preparation method, comprises the following steps: A) halogenated acetate with 2, 4 - dichlorophen salt reaction, to obtain 2, 4 - dichlorophenoxy ester; B) 2, 4 - dichlorophenoxy ester under the effects of catalyst hydrolysis reaction, to obtain 2, 4 - dichloro acid; said catalyst is selected from a polyether, a crown ether, quaternary ammonium salt, tertiary amine, [...], pyridine, titanate, inorganic acid, in organic acid one or more. The invention by halogenated acetate with 2, 4 - dichlorophen salt obtained by reaction of 2, 4 - dichlorophenoxy ester, and then in particular under the action of catalyst by hydrolysis reaction of the 2, 4 - dichloro acid. The invention specific reaction line combined with a specific catalyst such that the final preparation to obtain 2, 4 - dichlorophenoxyacetic acid purity and yield is relatively high, few by-products, the reaction route is simple, and is favorable for application. (by machine translation)
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Paragraph 0046; 0047
(2018/09/08)
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- Preparation method for 2,4-dichlorophenoxyacetic acid
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The invention provides a preparation method for 2,4-dichlorophenoxyacetic acid. The preparation method comprises the following steps: A) reacting C2 or above-C2 alcohol with halogenated acetic acid soas to obtain halogenated acetate; B) reacting halogenated acetic acid with 2,4-dichlorophenolate so as to obtain 2,4-dichlorophenoxyacetate; and C) hydrolyzing 2,4-dichlorophenoxyacetate so as to obtain 2,4-dichlorophenoxyacetic acid. According to the invention, C2 or above-C2 alcohol reacts with halogenated acetic acid to obtain a halogenated acetate intermediate, the intermediate has good stability, few reaction by-products are produced, and high yield is realized; then the intermediate further reacts with 2,4-dichlorophenolate to obtain 2,4-dichlorophenoxyacetate; and finally, 2,4-dichlorophenoxyacetate is hydrolyzed to obtain 2,4-dichlorophenoxyacetic acid. Through a specific reaction route of the invention, the finally prepared 2,4-dichlorophenoxyacetic acid has high purity and yield, few by-products are produced, the reaction route is simple, and the application of the preparation method is facilitated.
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Paragraph 0052; 0053; 0059; 0065
(2018/09/08)
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- A method for preparing 2, 4 - dichlorophenoxyacetic acid (by machine translation)
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The invention provides a 2, 4 - dichlorophenoxyacetic acid preparation method, comprises the following steps, first alcohol and a halogenated acetic acid after the reaction, to obtain halogenated acetate; the 2, 4 - dichlorophen after reaction with the alkali, to obtain 2, 4 - II [...]; then the above-mentioned step to obtain the halo acetate with 2, 4 - dichlorophen salt, to obtain 2, 4 - dichlorophenoxy ester; then obtained the above-mentioned step 2, 4 - dichlorophenoxy ester hydrolytic reaction, to obtain the 2, 4 - dichloro acid and alcohol; finally the above-mentioned step returns mellowly obtained is used in the aforesaid step, recycling; the alcohol is C atom number greater than or equal to 2 alcohol. The invention adjusts the process route, from the improved on the basis of, the reaction process is cleaning, of the small amount of waste water, hydrolysis few by-products, high purity of the product, the conversion and yield higher; and process raw materials can be recycled, is suitable for large-scale industrial production. (by machine translation)
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Paragraph 0012; 0092; 0094; 0095
(2018/09/08)
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- Preparation method for 2,4-dichlorophenoxyacetic acid
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The invention provides a preparation method for 2,4-dichlorophenoxyacetic acid, belonging to the technical field of organic synthesis. The preparation method comprises the following steps: a) reactinghalogenated acetate with 2,4-dichlorophenolate in the presence of a phase-transfer catalyst so as to obtain 2,4-dichlorophenoxyacetate; and b) hydrolyzing 2,4-dichlorophenoxyacetate so as to obtain 2,4-dichlorophenoxyacetic acid. According to the invention, oil-phase halogenated acetate reacts with 2,4-dichlorophenolate under the action of the phase-transfer catalyst to prepare 2,4-dichlorophenoxyacetate, and then 2,4-dichlorophenoxyacetate is hydrolyzed to obtain 2,4-dichlorophenoxyacetic acid and corresponding alcohols. Under the action of the phase-transfer catalyst, few hydrolysis by-products are produced during a reaction, fast reaction speed and high conversion rate and yield are obtained, and the amount of produced waste water is low; so industrial application of the preparation method can be easily implemented.
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Paragraph 0055; 0057; 0058
(2018/09/08)
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- Chloracetate water phase synthesis technology and novel method for preparing 2,4-D ester
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The invention discloses a chloracetate water phase synthesis technology and a novel method for preparing 2,4-D ester, and belongs to the technical field of organic synthesis. According to the chloracetate water phase synthesis technology, alcohol and chloroacetic acid are used as raw materials for preparing chloracetate in the water phase. The method for preparing 2,4-D ester comprises the following steps that (1) chloracetate is prepared; (2) 2,4-dichloroindophenol sodium is prepared; (2) the chloracetate directly takes a reaction with 2,4-dichloroindophenol sodium under the alkaline condition to obtain the corresponding 2,4-D ester. The operation of the preparation method of the chloracetate provided by the invention is performed in the water phase, so that the purity of the obtained coarse ester is higher, and can reach 99.3 percent or higher only through simple distillation; the corresponding 2,4-D ester is prepared from the chloracetate; the preparation process of the 2,4-D ester is greatly simplified; the cost is effectively reduced; the reaction time is greatly shortened; in addition, the product yield is improved; the waste water quantity is effectively reduced; the green chemical industrial requirements are met.
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Paragraph 0046; 0048
(2017/08/25)
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