- Research and development of the catalytic oxidation of methylacrylate to 3,3-dimethoxy methyl propionate
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A selective synthesis of 3,3-dimethoxy methyl propionate has been developed using a green approach, in which the key step is a palladium-catalyzed oxidation of methylacrylate in methanol using oxygen as oxidant. The relationship between several reaction p
- Tanaka, Yoshiyuki,Takahara, Jun P.,Lempers, Hans E.B.
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- Preparation method of methyl 3-methoxyacrylate
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The invention discloses a preparation method of methyl 3-methoxyacrylate. The preparation method comprises the steps: taking saturated monocarboxylic ester as a raw material and saturated carboxylic ester as an auxiliary material, and introducing formyl by utilizing methyl formate under the action of a catalyst; carrying out aldol condensation reaction with methanol under the condition that the ionic liquid is used as a catalyst, to obtain methyl 3,3-dimethoxypropionate; after the reaction is completed, separating methanol under reduced pressure, after separation is completed, increasing the temperature to 80-150 DEG C, carrying out an elimination reaction to remove one molecule of methanol on methyl 3,3-dimethoxypropionate, and thus obtaining methyl 3-methoxyacrylate, wherein methyl formate can be replaced with CO, and the raw material cost is lower. The method has the advantages of simple operation, easily available raw materials, high conversion rate, safety, environmental protection and low cost, and can realize industrial production.
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Paragraph 0086-0112
(2020/06/05)
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- Preparation method of methyl 3-methoxyacrylate
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The invention relates to a synthetic method of methyl 3-methoxyacrylate. The method is characterized by comprising the following steps that: (1) methyl 3, 3-dimethoxypropionate is synthesized from ketene dimer and trimethyl orthoformate at 25-90 DEG C under the catalytic action of an alkaline substance by taking alcohols as a solvent, and the molar ratio of the ketene dimer to trimethyl orthoformate to the alkaline substance is controlled to be 1: (1.0-5.0): (0.5-5.0); and (2) after the reaction is finished, the methyl 3, 3-dimethoxypropionate is cracked under the action of a catalyst to generate 3-methoxy methyl acrylate, and controlling the molar ratio of the methyl 3, 3-dimethoxypropionate to the catalyst to be 1: (1.0-5.0) and the reaction temperature to be 100-200 DEG C. According tothe method, raw materials are cheap and easy to obtain; the synthesis method is simple to operate; the reaction conditions are mild; requirements on equipment are low; and requirements of industrial large-scale production are met.
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Paragraph 0020-0026
(2020/12/10)
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- Method for preparing E-alkoxyacrylate through one-pot synthesis technology
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The invention discloses a method for preparing E-alkoxyacrylate through a one-pot synthesis technology. The method comprises the following steps: S1, carrying out a Friedel-Crafts reaction on alkenylether and oxalyl chloride; S2, decarboxylating a Friedel-Crafts reaction product obtained in step S1 to obtain alkenyl acyl chloride; and S3, esterifying the alkenyl acyl chloride to obtain the E-alkoxyacrylate. The alkenyl ether and oxalyl chloride undergo the Friedel-Crafts reaction at a low temperature under solvent-free and metal catalyst-free conditions, the Friedel-Crafts reaction product undergoes heating decarboxylation to obtain the alkenyl acyl chloride, and the alkenyl acyl chloride is esterified to obtain the E-alkoxyacrylate, so precious metal catalysts and a lot of solvents are not used in the whole technologic route, and severely toxic phosgene and expensive initial raw materials are avoided, thereby the technologic route has the cost advantage in industrial amplified production.
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Paragraph 0044; 0050; 0054; 0058; 0062; 0063; 0066; 0070
(2018/07/06)
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- Preparation process of MAME (methyl 3-methoxyacrylate)
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The invention provides a preparation process of MAME (methyl 3-methoxyacrylate) and belongs to the technical field of synthesis of organic compounds. According to the preparation process, methyl acrylate and excess methanol taken as starting raw materials are subjected to an addition-etherification reaction in an oxygen atmosphere under the action of a synthetic catalyst, a product is subjected tofiltration and extraction, methyl 3,3-dimethoxypropionate is obtained and subjected to a catalytic cracking reaction, MAME and methanol are generated, the target product MAME is obtained through distillation, and methanol is recovered, wherein the synthetic catalyst is cobalt oxide, indium oxide or a mixture of cobalt oxide and indium oxide in any proportion. The preparation process is simple andefficient, the yield of the product MAME is higher and reaches 78%-82.4%, the catalyst can be recycled for a long time, corrosive and toxic substances are avoided, reaction equipment cannot be corroded, industrial production can be realized, and considerable economic benefits are created.
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Paragraph 0016-0020
(2018/04/26)
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- Synthesizing method for 3-methoxyacrylate
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The present invention relates to a synthesizing method for 3-methoxy-3-ethoxy methyl propionate, and belongs to the field of chemistry. The synthesizing step comprises the following steps: introducing methyl vinyl ether into trichloroacetyl chloride, and insulating until a reaction is completed; combining BJ01 with anhydrous methanol, adding an acid-binding agent I, and insulating until a reaction is completed; and mixing BJ02 with an organic solvent 2, adding a catalyst, and insulating until a reaction is completed to obtain the 3-methoxyacrylate. The synthesizing method for the 3-methoxyacrylate has the advantages of few reaction steps, easiness in operation, less waste gas, waste water and waste residues, high yield, high purity of products, and inexpensive and easily available raw materials. All the steps have no harsh conditions and are simple in operation and environmentally-friendly, and the solvent are easily recycled and reused, so that the synthesizing method is suitable for industrial production.
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Paragraph 0020; 0023
(2016/10/17)
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- PROCESS FOR THE PREPARATION OF ALKYL 3,3-DIALKOXYPROPIONATES
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The present invention relates to a continuous process for preparing alkyl 3,3-dialkoxy-propionates of the formula (RO)2CHCH2CO2R, wherein R is C1-6 alkyl, by reacting ketene with an ortho formate of formula (RO)3CH in the presence of an acidic catalyst, characterized in that the reaction is carried out in a loop reactor.
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Page/Page column 8-9
(2009/06/27)
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- Pd(II)-catalyzed acetalization of terminal olefins with electron-withdrawing groups in supercritical carbon dioxide: selective control and mechanism
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Pd(II)-catalyzed acetalization of terminal olefins with electron-withdrawing groups was carried out smoothly in supercritical carbon dioxide under oxygen atmosphere when polystyrene-supported benzoquinone (PS-BQ) or CuII (CuI) chloride was employed as cocatalyst. The higher selectivity was achieved, without any chlorinated by-product detected, when using PS-BQ instead of CuII (or CuI) chloride. PS-BQ could be recycled with excellent catalytic activity remaining after each simple filtration. Chlorine ion was demonstrated to be a promoter. The different acetalization mechanisms were revealed by the subtle relationship of chlorine ion and benzoquinone (BQ) to the catalytic activity of PdCl2/PS-BQ, PdII-CuCl2 or Pd(OAc)2/PS-BQ.
- Wang, Zhao-Yang,Jiang, Huan-Feng,Ouyang, Xiao-Yue,Qi, Chao-Rong,Yang, Shao-Rong
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p. 9846 - 9854
(2007/10/03)
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- The Allopolarization Principle and its Applications, IV. Substituent Effects in the Methylation of Enolate Anions
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The ratio of O- and C-methylated products in the reaction of the sodium salts of acetophenones 1, propiophenones 3, phenylacetones 5, β-dicarbonyl compounds 12, α-cyanocarbonyl compounds 13, acetaldehyde, propionaldehyde, and diethylketone with dimethyl sulfate, methyl iodide, and trimethyl phosphate in HMPTA has been determined with regard to the effect of substituents.In some cases the influence of solvents, concentration and temperature has also been studied.
- Gompper, Rudolf,Vogt, Hans-Hubert
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p. 2866 - 2883
(2007/10/02)
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