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7424-91-1Relevant articles and documents
Ozonolysis of α-angelica lactone: a renewable route to malonates
Dell’Acqua, Andrea,Stadler, Bernhard M.,Tin, Sergey,Wille, Lukas,de Vries, Johannes G.
supporting information, p. 10524 - 10527 (2021/10/19)
Industrially relevant intermediates such as malonic acid, malonates and 3-oxopropionates can be easily accessed by ozonolysis of α-angelica lactone, derived from the platform chemical levulinic acid. The roles of the solvent and of the quenching conditions are of key importance for the outcome of the reaction.
Green preparation method of uracil
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Paragraph 0025, (2021/01/25)
The invention relates to a green preparation method of uracil, which comprises the following steps: proportionally mixing acetate, alkali and a benzene solvent in a reaction bottle to obtain a mixed solution, introducing carbon monoxide, pressurizing to generate aldehyde, adding a hydrogen chloride alcohol solution into the reaction bottle, and carrying out condensation reaction on aldehyde and the hydrogen chloride alcohol solution to obtain acetal, and adding urea into the reaction bottle, reacting acetal with urea to obtain a condensate, adding alkali into the reaction bottle, reacting alkali with the condensate to generate uracil sodium salt, adding acidic water into the reaction bottle, crystallizing, cooling, and filtering to obtain uracil. Carbon monoxide and acetate are innovatively used as raw materials, alkali such as sodium methoxide is used for one-pot catalytic synthesis of uracil, the synthesis method in the whole process is mild in condition, simple in process and high in yield and purity, the purposes of few three wastes and environmental protection are achieved, and the method has a good large-scale application prospect.
Preparation method of methyl 3-methoxyacrylate
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Paragraph 0020-0026, (2020/12/10)
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.
Preparation process of MAME (methyl 3-methoxyacrylate)
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Paragraph 0016-0020, (2018/04/26)
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.
Preparation method of 3,3-dialkoxylpropionate
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Paragraph 0029; 0033; 0037, (2017/09/02)
The invention belongs to the technical field of preparation of drug intermediates and in particular relates to a preparation method of 3,3-dialkoxylpropionate. The preparation method comprises the following steps: firstly, taking alkyl vinyl ether and trichloroacetyl chloride as raw materials; reacting under a certain condition to obtain an intermediate product 1,1,1-trichloro-4-alkoxyl-3-butene-2-one; reacting under an alkaline condition to obtain a target product 3,3-dialkoxylpropionate. The preparation method of the 3,3-dialkoxylpropionate, provided by the invention, has the following active effects that one raw material is directly used as a solvent (trichloroacetyl chloride) to react and the recycling and consumption of the solvent in a production process are reduced to a certain extent; after the reaction, an alcohol solvent can be recycled and is used for reacting for the next time, so that the recycling is realized and the scheme meets the requirements of green chemistry; a preparation process is simple, low in energy consumption and low in cost and can be in mass production.
Atom-economical synthesis of 3,3,3-trifluoropropanal dialkyl acetals through Pd/C catalyzed acetalization of 3,3,3-trifluoropropene
Kang, Jian-Ping,Lu, Ju-You,Li, Yang,Wang, Zhi-Xuan,Mao, Wei,Lu, Jian
, p. 39387 - 39391 (2016/06/01)
A facile and efficient procedure for one-step synthesis of 3,3,3-trifluoropropanal dialkyl acetals from readily available 3,3,3-trifluoropropene (TFP) has been developed. The catalyst can be recycled for 4 times without obvious deactivation. This process provides a novel and atom-economical synthetic strategy for the preparation of functional CF3-containing compounds.
Synthesizing method for 3-methoxyacrylate
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Paragraph 0019; 0025, (2016/10/17)
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.
Acid-catalyzed oxidation of levulinate derivatives to succinates under mild conditions
Wang, Yuran,Vogelgsang, Ferdinand,Román-Leshkov, Yuriy
, p. 916 - 920 (2015/03/18)
Levulinate derivatives are an attractive platform for the production of renewable chemicals. Here we report on the oxidation of methyl levulinate into dimethyl succinate with peroxides under mild conditions using Br?nsted and Lewis acid catalysts. Selectivities to succinate and acetate derivatives of approximately 60 and 40 %, respectively, were obtained with strong Br?nsted acids in methanol. Although the molecular structure (i.e., carbon-chain length and branching around the C=O group) and the oxidant type affect the product distribution, solvent choice has the strongest impact on changing the location of oxygen insertion into the carbon backbone. Specifically, switching the solvent from methanol to heptane resulted in a decrease in the succinate/acetate ratio from 1.6 to 0.3. In contrast to Br?nsted acids, we demonstrate that the nature of the metal cation is responsible for changing the reaction selectivity of water-tolerant Lewis acidic triflate salts.
Catalytic oxidative decarboxylation of malic acid into dimethyl malonate in methanol with dioxygen
Liu, Junxia,Du, Zhongtian,Yang, Yanliang,Lu, Tianliang,Lu, Fang,Xu, Jie
, p. 2151 - 2154 (2013/01/15)
If you've got it, use it: Malic acid is converted into dimethyl malonate by a direct, one-pot process. The process is cyanide- and halide-free. Phosphovanadomolybdates serve as bifunctional catalysts, effecting the oxidative decarboxylation and esterification in a consecutive manner. Oxidative C-C bond cleavage first forms hemiacetals. The results serve as example for the production of valuable chemicals by fully utilizing the oxygen atoms and basic structure inherent to biomass products.
Research and development of the catalytic oxidation of methylacrylate to 3,3-dimethoxy methyl propionate
Tanaka, Yoshiyuki,Takahara, Jun P.,Lempers, Hans E.B.
experimental part, p. 548 - 554 (2010/04/22)
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
