50650-75-4Relevant academic research and scientific papers
Preparation process of pyridinone ethanol amine salt
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, (2021/01/25)
The invention relates to the technical field of pyridone ethanol amine salt processing, and particularly discloses a pyridone ethanol amine salt preparation process, which comprises: carrying out an acylation reaction, a ring-closure reaction, a hydroxyamination reaction and a salt forming reaction on 3,3-dimethyl acrylate and isononyl chloride to obtain pyridone ethanol amine salt; wherein the acylation reaction is carried out in the presence of a supported catalyst, the supported catalyst comprises an active component and a carrier, the carrier is silica gel, the active component comprises anhydrous aluminum chloride, anhydrous lanthanum chloride and anhydrous lithium perchlorate, and the loading capacity of anhydrous aluminum chloride on the carrier is 7-11 wt%; the loading capacity ofanhydrous lanthanum chloride on the carrier is 3-5 wt%; and the loading capacity of anhydrous lithium perchlorate on the carrier is 0.8-1.5 wt%. According to the preparation process of pyridinone ethanol amine salt, the catalytic Friedel-Crafts acylation reaction is realized, the supported catalyst is convenient to recover, and the activity and selectivity of the supported catalyst are improved.
Synthetic method 4 - methyl - (2, 4, 4 -trimethylpentyl) - 2H - pyran -2 - ketone
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Paragraph 0028; 0030-0031; 0033-0034; 0036-0037; 0039; ..., (2021/10/13)
The invention discloses a synthetic method of 4 - methyl - (2, 4, 4 -trimethylpentyl) - 2H - pyran -2 - ketone, which comprises the following steps S1: taking 3 and 3 - dimethyl acrylate. The isononyl chloride is taken as a raw material, dichloromethane is taken as a solvent, and a Fourier acylation reaction is carried out under the action of a Lewis acid to obtain the intermediate M1. S2: The intermediate M1 is added to the reaction vessel, the organic solvent is added for stirring and dissolving, calcium oxide is added to the 20 - 120 °C-down ring reaction, and cooling is carried out. The target product is obtained by filtration and purification. The reaction conditions are mild, the synthetic route is short, pollution is avoided, the product purity is high 20 -120 °C, the yield is high, and the problems of complex route, difficult operation, high danger, high cost, pollution and low yield of an existing oxypyridone intermediate are solved.
Preparation method of pyridinone ethanolamine salt
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, (2020/03/05)
The invention discloses a preparation method of a pyridinone ethanolamine salt. The preparation method comprises the reaction steps of Friedel-Crafts acylation, ring closing, hydroxyamination, salification and the like. According to the preparation method, the pyridinone ethanolamine salt can be efficiently prepared under mild conditions, less reaction materials are consumed, the yield and purityof products obtained in the steps are high, and complex purification steps are not needed.
4-methyl-6-(2,4,4-trimethylpentyl)-2-pyrone preparation method
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Paragraph 0017; 0019-0021; 0023-0025; 0027; 0028, (2020/03/02)
The invention relates to a method for preparing 4-methyl-6-(2,4,4-trimethylpentyl)-2-pyrone. According to the invention, methyl 3-methyl-2-butenoate and isononanoyl chloride are subjected to a reaction in presence of aluminum chloride (aluminum chloride and isononanoyl chloride are complexed to serve as a coordination catalyst) to generate diketone ester, wherein the heat released by the reactionis fully utilized (ice bath is not adopted, and the temperature is adjusted to 10-80 DEG C according to the natural temperature), so that the use of cooling capacity and heat is reduced, and the costis saved; in a reaction liquid quenching process, the hydrochloric acid prepared by absorbing the tail gas HCl generated in the reaction process by water is fully utilized, so that the use of concentrated hydrochloric acid and process water is reduced, and the waste liquid is reduced so as to save the cost; and crude 4-methyl-6-(2,4,4-trimethylpentyl)-2-pyrone is purified in a reduced pressure distillation mode, so that the treatment of three wastes is reduced, the obtained 4-methyl-6-(2,4,4-trimethylpentyl)-2-pyrone product is high in purity and light in color, and the method is beneficial tosynthesis and preparation of downstream products.
Two-step method for synthesis of 4-methyl-6-(2,4,4-trimethylpentyl)-2H-Pyran-2-ketone
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Paragraph 0021-0026, (2019/11/12)
The invention relates to the technical field of synthesis of chemical intermediates, in particular to a two-step method for the synthesis of 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-ketone. The two-step method is a two-step synthesis method, and includes the steps that isononyl chloride and 3,3- dimethacrylate are used as raw materials, and acylation reaction is carried out on a catalyst of anhydrous aluminum trichloride to synthesize 3,7,9,9-tetramethyl-2-decene-5-ketoacid methyl ester; then, under the catalysis of concentrated sulfuric acid, cyclization reaction is carried out with glacial acetic acid, and the product is obtained by purifying. Compared with other process routes, the two-step method is less in reaction steps, high in yield, high in product purity, low in production cost, less in equipment requirements, and is suitable for industrial production.
