- Production method of 2-propoxyethyl chloride
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The invention relates to a production method of 2-propoxyethyl chloride and belongs to the technical field of fine chemical intermediate organic synthesis. The synthesis process comprises the following steps: preparing a crude product by taking ethylene glycol monopropyl ether and excessive sulfoxide chloride as main raw materials and adopting an efficient catalyst through heating and heat preservation, wherein the reaction rate is controlled by dropwise adding sulfoxide chloride; and performing neutralization, hydrolysis, and liquid separation after standingto obtain 2-propoxyethyl chloride. Compared with the existing process, the synthesis process has the advantages that the catalyst has higher catalytic efficiency and is cheap and easily available; the technological process is simple and convenient; the catalyst used in the existing process and hydrochloric acid in the crude product form a complex easily, so that the product has precipitates and the product yield is influenced; and the crude product prepared by the catalyst is clear and transparent, the product can be obtained without water washing, the quality is stable, the product content reaches above 99.5 percent, the yield is more than 99.0 percent, the production cost is lower, and the synthesis process is particularly suitable for industrialized production.
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Paragraph 0012; 0017-0032
(2017/08/30)
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- Synthesis process of 2-propoxyethyl chloride
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The invention relates to a synthesis process of 2-propoxyethyl chloride and belongs to the technical field of fine chemical intermediate organic synthesis. The synthesis process comprises the following steps: preparing a crude product by taking ethylene glycol monopropyl ether and excessive sulfoxide chloride as main raw materials and adopting an efficient catalyst through heating and heat preservation, wherein the reaction rate is controlled by dropwise adding sulfoxide chloride; and performing neutralization, hydrolysis, and liquid separation after standing to obtain 2-propoxyethyl chloride. Compared with the existing process, the synthesis process has the advantages that the catalyst has higher catalytic efficiency; and the existing process needs 0.1 to 0.2 mol of excessive sulfoxide chloride, but the catalyst only needs 0.01 mol of excessive sulfoxide chloride, so fewer waste water and waste residues are generated when the crude product is treated, the product content reaches above 99.5 percent, the yield is more than 99.0 percent, the production cost is lower, and the synthesis process is suitable for industrialized production.
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Paragraph 0012; 0017-0032
(2017/08/30)
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- Preparation process of 2-propoxy chloroethane
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The invention relates to a preparation process of 2-propoxy chloroethane and belongs to the technical field of organic synthesis of fine chemical intermediates. The synthetic process comprises the following steps: by taking ethylene glycol monopropyl ether and excess thionyl chloride as raw materials and adopting a high efficiency composite catalyst, controlling the reaction rate through dropwise adding the thionyl chloride, raising the temperature and preserving the temperature to obtain a crude product, neutralizing, hydrolyzing, standing and layering to obtain the 2-propoxy chloroethane. Compared with the prior art, the preparation process disclosed by the invention has the advantages that the catalyst is higher in catalytic efficiency, low in price and easy to get; the process is simple, safe and reliable; the product is high in yield and stable in quality; the product content is up to above 99.0%; the yield is greater than 98.5%; catalysts used in the prior art easily react with little hydrochloric acid contained in the product to form complex salt which is a precipitate in the 2-propoxy chloroethane and then the product quality is influenced; and the preparation process is particularly suitable for industrial production.
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Paragraph 0016; 0017; 0018; 0019; 0020; 0021; 0022-0031
(2017/09/02)
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- Preparation method of chloro-aliphatic ether
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The invention discloses a preparation method of chloro-aliphatic ether, and aims to solve the problems that when 2-propoxy-dichloroethane is synthesized by adopting an existing method, a large amount of sulphur dioxide is produced and the amount of wastewater is large, solid waste pollution can be produced if a phase catalyst is recycled and applied mechanically, and when triphosgene is used as a chlorating agent, the price of the triphosgene is expensive so that the triphosgene is not suitable for large-scale industrial production. The method comprises the following steps: 1) carrying out reaction on a compound shown in a formula (I) and carbonyl chloride to prepare a compound shown in a formula (II); (2) carrying out decarboxylic reaction on the compound shown in the formula (II) to prepare a compound shown in a formula (III). According to the preparation method disclosed by the invention, a brand-new route for preparing the chloro-aliphatic ether is provided, so that the yield of the chloro-aliphatic ether is high, and the production cost can be effectively reduced; moreover, HC1, CO2 and a small amount of high-salinity wastewater only can be produced, so that three wastes are little, the environment protection is achieved, and the environment protection cost is low; in addition, the method also can be applied to preparation of multi-structure chloro-aliphatic ether, has a higher application value and wide application prospect, and is worthy of massively popularized and applied.
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Paragraph 0099; 0112; 0117-0118; 0124; 0129; 0130
(2017/10/13)
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- Preparation method of chloroformate derivatives, and application of preparation method
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The invention discloses a preparation method of chloroformate derivatives, and application of the preparation method, belonging to the field of chemical synthesis. The invention aims at providing a new preparation method, which can meet the needs of industrial production, of the chloroformate derivatives. The chloroformate derivatives prepared by the method are as shown in a formula (II) below; the method comprises the following step: enabling compounds as shown in a formula (I) to react with phosgene so as to obtain the compounds shown in the formula (II), wherein a reaction equation is shown in the description. The preparation method provided by the invention has the advantages of simple and convenient production, safety and the like; the prepared product has higher product purity and reaction yield; furthermore, the treatment of three wastes is simple and convenient; therefore, the preparation method has higher application value and wide application prospect and is worth large-scale popularization and application.
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Paragraph 0106; 0108-0115; 0117-0119; 0120-0125
(2017/11/18)
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- Method for synthesizing 2-chloroethyl-propylether
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The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing 2-chloroethyl-propylether. An efficient nucleophilic catalyst is adopted, 2-propoxyethanol and thionyl chloride serve as main raw materials, the reaction speed is strictly controlled by adding thionyl chloride dropwise, and then a crude product is obtained after heating and heat preserving; after cooling, solid alkali is directly added to decompose excessive thionyl chloride and neutralize thionyl chloride; finally, 2-chloroethyl-propylether is obtained after filtering. The purity reaches 99.5% or above, the yield is larger than 98.8%, and the water content is smaller than 0.1%. Compared with the prior art, no waste water is generated, the purity and the yield are high, water content is low, and the method is economical, environmentally friendly and suitable for industrial production.
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Paragraph 0036-0038
(2017/03/14)
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- Preparation method of chloroethyl-n-propylether
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The invention relates to the technical field of organic synthesis and concretely relates to a preparation method of chloroethyl-n-propylether. 2-n-propoxyethanol and thionyl chloride as main raw materials undergo a reaction in the presence of a high-efficiency nucleophilic catalyst, wherein through dropwise addition of thionyl chloride, a reaction rate is strictly controlled, the product is heated and is subjected to thermal insulation to form a crude product, and the crude product is subjected to rectification purification to form chloroethyl-n-propylether. The product has clear and transparent appearance, purity of 99.2% or more, a yield of 98.5% or more and water content of 0.2% or less. Compared with the traditional technology, the preparation method does not produce waste water, realizes recycle of a front cut fraction and kettle bed material produced by rectification and a catalyst, realizes high purity, high yield and low water content and is suitable for industrial production.
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Paragraph 0009; 0036; 0037; 0038
(2016/10/20)
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- Preparation method of 1-(2-chloroethoxy)propane
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The invention belongs to the field of organic synthesis technology, and concretely relates to a preparation method of 1-(2-chloroethoxy)propane. Under the synergistic effect of a plurality of catalysts, 2-propoxyethanol and thionyl chloride are used as main raw materials, reaction rate is controlled by adding thionyl chloride drop by drop, heating and insulation are carried out, and a crude product is obtained; hydrolysis and neutralization are carried out, a mixture is permitted to stand for separation, and 1-(2-chloroethoxy)propane is obtained. Compared with prior art, the catalysts are cheap and easily available, the catalysis efficiency is higher, the process is simple with safety and reliability, the product yield is high, the quality is stable, the product content reaches above 99.0%, the yield is higher than 98.5%, the production cost is low, and the method is especially suitable for industrial production.
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Paragraph 0010; 0028; 0029; 0030
(2016/10/27)
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- Preparation method of 1-(2-chloroethoxy)propane
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The invention belongs to the technical field of organic synthesis and specifically relates to a preparation method of 1-(2-chloroethoxy)propane. By an efficient nucleophilic catalyst, 2-propoxyethanol and thionyl chloride are used as main raw materials, and reaction temperature is strictly controlled by dropwise adding thionyl chloride; after heating and thermal insulation, a crude product is obtained; and after hydrolysis, neutralization and standing for liquid separation, 1-(2-chloroethoxy)propane is obtained. In comparison with traditional technologies, the invention has the following advantages: efficiency of the catalyst is higher; the technological process is safe and reliable; operation is simple; product yield is high; quality is stable; product content reaches 99.0% and above; yield is greater than 98.5%; and production cost is lower. The preparation method of the invention is especially suitable for industrial production.
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Paragraph 0010; 0036; 0037; 0038
(2016/11/24)
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- Synthetic method of 1-(2-chloroethoxy)propane
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The invention belongs to the technical field of organic synthesis and specifically relates to a synthetic method of 1-(2-chloroethoxy)propane. Under the action of a phase-transfer catalyst, 2-propoxyethanol and thionyl chloride are used as main raw materials, and reaction rate is controlled by dropwise adding thionyl chloride; after heating and thermal insulation, a crude product is obtained; and after hydrolysis, neutralization and standing for liquid separation, 1-(2-chloroethoxy)propane is obtained. In comparison with prior art, catalytic efficiency of the catalyst is high, the technological process is simple, safe and reliable, product yield is high, quality is stable, product content reaches 99.0% and above, yield is greater than 98.5%, and production cost is lower. The synthetic method of the invention is especially suitable for industrial production.
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Paragraph 0025; 0027; 0028; 0029
(2016/12/12)
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- Synthetic method for 2-propoxyethyl chloride
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The invention belongs to the technical field of organic synthesis and particularly relates to a synthetic method for 2-propoxyethyl chloride. According to the synthetic method, an efficient catalyst is adopted, 2-propoxyethanol and thionyl chloride are adopted as main raw materials, by dripping thionyl chloride, the reaction rate is controlled strictly, the temperature is raised and preserved so that a crude product can be obtained, and rectifying purification is carried out to obtain 2-propoxyethyl chloride. The product is clear and transparent in appearance, purity is 99.4% or more, the yield is larger than 98.6%, and the water content is smaller than 0.18%. Compared with a traditional technology, no waste water is generated, fore distillate, kettle bed charge and the catalyst generated by rectification can be recycled, the purity and the yield are high, the water content is low, and the synthetic method is suitable for industrialized production.
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Paragraph 0009; 0031; 0036-0038
(2017/03/08)
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- Compounding technology of chloroethyl n-propyl ether
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The invention belongs to the technical field of organic syntheses, and specifically relates to a compounding technology of chloroethyl n-propyl ether. The compounding technology comprises the steps of adopting an efficient catalyst taking 2-n-propoxyl ethyl alcohol and thionyl chloride as main raw materials; strictly controlling the reaction speed by dripping the thionyl chloride; obtaining a crude product through temperature rising and temperature preservation; obtaining the chloroethyl n-propyl ether through rectification and purification. The product appearance is clear and transparent, the purity is more than 99.22 percent, the yield is greater than 98.53 percent, and the water content is smaller than 0.19 percent; compared with the prior art, no wastewater is generated, fore-distillate and a kettle bottom material which are generated by rectification and the catalyst can be recycled, the purity and the yield are high, the water content is low, and the compounding technology is suitable for industrial production.
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Paragraph 0009; 0028; 0029; 0030
(2016/11/28)
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- Synthesis process of 2-propoxy-chloroethane
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The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis process of 2-propoxy-chloroethane. The synthesis process comprises the steps that ethylene glycol mono-n-propyl ether and thionyl chloride are used as main materials under the synergistic effect of multiple catalysts; the reaction temperature is controlled by dropwise adding the thionyl chloride; a crude product is obtained through temperature rise and heat preservation; solid alkali is directly added after cooling to resolve excessive thionyl chloride and neutralization is performed; the 2-propoxy-chloroethane is finally obtained through filtration. Compared with the existing process, the synthesis process of the 2-propoxy-chloroethane has the advantages that the catalysts are low in price, easy to obtain, the catalytic efficiency is higher, the technological process is simple and convenient, safe and reliable, the product yield is high and the quality is stable, and the product content reaches 99.2 percent or more, the yield is greater than 98.6 percent, the product cost is lower, and the synthesis process of 2-propoxy-chloroethane is particularly suitable for industrial production.
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Paragraph 0010; 0032; 0033; 0034
(2016/10/08)
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- Studies on the Mechanism of the Chlorohydrination of Olefins
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We studied the rate-determining and the product-determining steps of the chlorohydrination of olefins with Cl2/H2O and HOCl.In competitive kinetic experiments with 3-ethylpent-2-ene and cyclohexene we determined the relative rate constants krel=1,5 (with Cl2/H2O) and krel=infinite (with HOCl).This shows that the rate-determining steps of the chlorohydrination with Cl2/H2O and with HOCl are different.In order to investigate the product-determining steps we determined the proportion of alkyl-(2-chloroethyl)-ethers 3 and ethylene chlorohydrine 2 in the reaction of ethylene with Cl2 and with HOCl in alcohol/water-mixtures.The proportion of both the reaction products 3/2 was independent of the chlorinating agent used.Also the proportion of MARKOVNIKOV and anti-MARKOVNIKOV products in the chlorohydrination of propylene with Cl2/H2O or HOCl was independent of the type of chlorinating agent.In the chlorohydrination of cyclohexene both agents (Cl2/H2O and HOCl) yielded only the trans-chlorohydrine.From the results obtained it may be concluded that the product-determining step of chlorohydrination is the same for both the chlorinating agents studied.
- Buss, E.,Rockstuhl, A.,Schnurpfeil, D.
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p. 197 - 208
(2007/10/02)
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