- Method for synthesizing straight-chain octadecanedioic acid
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The invention provides a method for synthesizing straight-chain octadecanedioic acid, which comprises the following steps of: carrying out double decomposition reaction on a compound shown in a formula (I) under the condition of a Grubbs catalyst to generate an unsaturated acid compound shown in a formula (II); and reducing the compound as shown in the formula (II) into a compound as shown in a formula (III) through palladium-carbon hydrogenation. The method disclosed by the invention is convenient to operate, simple in process, simple and easily available in raw materials and low in cost, and is suitable for small-scale preparation in a laboratory and industrial production.
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Paragraph 0028; 0029; 0031; 0032; 0033; 0035
(2022/03/27)
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- Preparation method of long-chain diacid
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The invention provides a preparation method of long-chain diacid, which comprises the following steps of: (S1) carrying out an addition reaction on olefine acid or an ester derivative thereof serving as a raw material and liquid bromine to obtain dibromo carboxylic acid or an ester derivative thereof; (S2) carrying out an elimination reaction on the dibromo carboxylic acid or ester derivative thereof under the action of sodium amide to obtain alkynyl-terminated carboxylic acid or an ester derivative thereof; (S3) carrying out an addition reaction on the alkynyl-terminated carboxylic acid or the ester derivative thereof and diborane to obtain borane or boric acid containing carboxyl or ester group; and (S4) oxidizing the borane or boric acid to obtain long-chain diacid. According to the invention, olefine acid is used as a raw material, is easily available in source and low in price, so that the production cost of the product is very low; and meanwhile, the raw materials used in the synthesis process do not contain precious metals or other expensive reagents, so that the synthesis process is suitable for industrial amplification production, and the defect that the method in the prior art is not environment-friendly, not suitable for industrial production and high in preparation cost is overcome.
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Paragraph 0050-0051; 0057-0059; 0080; 0087-0089
(2021/11/03)
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- Preparation method of long-chain aliphatic dicarboxylic acid mono-tert-butyl ester
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The invention provides a method for obtaining the long-chain aliphatic dicarboxylic acid mono-tert-butyl ester through monohydrolysis of the long-chain aliphatic dicarboxylic acid di-tert-butyl ester by controlling the reaction conditions of monohydrolysis; and the raw material cost is low, the yield is high, the post-treatment method is simple, and the method is suitable for industrial production.
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Paragraph 0040-0043
(2021/07/09)
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- Preparation method of long-chain alkyl diacid
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The invention relates to a preparation method of long-chain alkyl diacid, belonging to the technical field of organic synthesis. The method is characterized in that long-chain alkyl diacid is prepared by hydrolyzing a long-chain alkyl acid derivative serving as a starting raw material under an acidic condition. According to the invention, a novel synthesis route is adopted, raw material cost is reduced, and the synthesis method has the characteristics of mild reaction conditions, simple process operation, low production cost and the like, and shows good application prospects. The long-chain alkyl diacid serving as an intermediate for medicine synthesis has very high application value and very high economic value.
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Paragraph 0139; 0154-0161; 0162; 0177-0184; 0185; 0200-0207
(2021/06/12)
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- Preparation method of long-chain alkyl diacid mono-tert-butyl ester
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The invention relates to a preparation method of long-chain alkyl diacid mono-tert-butyl ester, belonging to the technical field of organic synthesis. According to the invention, long-chain alkyl diacid is used as an initial raw material and reacts with oxalyl chloride to generate long-chain monoacyl chloride, and the long-chain monoacyl chloride and tert-butyl alcohol are subjected to an esterification reaction to generate the long-chain alkyl diacid mono-tert-butyl ester. According to the invention, a novel synthesis route is adopted, and raw material cost is reduced; and the method has the characteristics of mild reaction conditions, simple process operation, high product purity, high production efficiency and the like, and has good application prospects.
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Paragraph 0192; 0208-0215; 0224; 0240-0247; 0256; 0271-0278
(2021/06/13)
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- Preparation method of octadecanedioic acid (by machine translation)
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The method has the advantages that raw materials are cheap and easily available, and 9 - McMMMMMurry Coupling forms a coupling intermediate; and then, the method is cheap and easily available in raw materials, simple in post-treatment steps, and capable of greatly reducing production cost and selling price of octadecanedioic acid. (by machine translation)
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Paragraph 0030; 0038-0042; 0043; 0052-0055; 0056; 0065-0067
(2020/07/12)
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- Preparation method of octadecanedioic acid
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The invention relates to a preparation method of octadecanedioic acid. The preparation method comprises the following steps: (1) in the presence of a catalyst and an organic solvent, carrying out freeradical coupling reaction on a compound shown in a formula I and butadiene at 30-90 DEG C to prepare octadecyl-7, 11-diene diacid; and (2) dissolving the octadecyl-7, 11-diene diacid prepared in thestep (1) in an alcohol solvent, introducing hydrogen under the action of a palladium-carbon catalyst, and carrying out a catalytic hydrogenation reaction at 30-50 DEG C to prepare the octadecanedioicacid, the specific synthesis route being shown in the specification. The method is adopted to prepare the octadecanedioic acid, the total yield of the target product reaches 85% or above, the purity reaches 98.5% or above, the synthesis steps are few, the reaction conditions are mild, and the method is suitable for large-scale production; the use of polluting heavy metals and toxic reagents is avoided, the cost is low, and the market prospect is wide.
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Paragraph 0012; 0033; 0036-0038; 0041-0043; 0046-0048; 0051
(2020/12/30)
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- Preparation method of surfactant
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The invention provides a preparation method of a surfactant, specifically comprising the following four steps: 1, preparing an intermediate 1 by using methyl oleate as a raw material; 2, letting the intermediate 1 firstly react with borane in a solvent, then oxidizing with hydrogen peroxide, and finally performing alkaline hydrolysis to obtain an intermediate 2; 3, jointly oxidizing the intermediate 2 into an intermediate 3 in a solvent by sodium hypochlorite, sodium perchlorate and TEMPO (2, 2, 6, 6-tetramethylpiperidine-1-oxy CAS number: 2564-83-2); and 4, hydrolyzing the intermediate 3 in asolvent under an alkaline condition, and acidifying to obtain the surfactant octadecanedioic acid. The preparation method is a synthetic method including four steps of chemical reactions, and can efficiently convert methyl oleate into octadecanedioic acid. The method is simple to operate; and the reagent is cheap and easily available, green and safe, efficient and environmentally-friendly, and suitable for industrial production.
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- Synthesis of Carboxylic Acids by Palladium-Catalyzed Hydroxycarbonylation
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The synthesis of carboxylic acids is of fundamental importance in the chemical industry and the corresponding products find numerous applications for polymers, cosmetics, pharmaceuticals, agrochemicals, and other manufactured chemicals. Although hydroxycarbonylations of olefins have been known for more than 60 years, currently known catalyst systems for this transformation do not fulfill industrial requirements, for example, stability. Presented herein for the first time is an aqueous-phase protocol that allows conversion of various olefins, including sterically hindered and demanding tetra-, tri-, and 1,1-disubstituted systems, as well as terminal alkenes, into the corresponding carboxylic acids in excellent yields. The outstanding stability of the catalyst system (26 recycling runs in 32 days without measurable loss of activity), is showcased in the preparation of an industrially relevant fatty acid. Key-to-success is the use of a built-in-base ligand under acidic aqueous conditions. This catalytic system is expected to provide a basis for new cost-competitive processes for the industrial production of carboxylic acids.
- Sang, Rui,Kucmierczyk, Peter,Dühren, Ricarda,Razzaq, Rauf,Dong, Kaiwu,Liu, Jie,Franke, Robert,Jackstell, Ralf,Beller, Matthias
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supporting information
p. 14365 - 14373
(2019/09/06)
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- HIGH PURITY DIBASIC ACID COMPOSITIONS AND METHODS OF MAKING THE SAME
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High-purity dibasic acid compositions are generally disclosed. In some embodiments, the dibasic acid compositions are solutions or suspensions. In some other embodiments, the compositions are solid-state compositions. In some such embodiments, the solid-state compositions include a dibasic acid as a crystalline solid and further include a low quantity of certain impurities, such as monobasic acids, various esters, and the like. Methods and systems for making such high-purity dibasic acid compositions are also disclosed.
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Paragraph 0190-0194
(2015/04/28)
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- PURIFICATION OF POLYCARBOXYLIC ACIDS
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A process for purifying a polycarboxylic acid from a mixture is provided. Optionally, the mixture is an aqueous solution and optionally the process comprises an acidification step and/or the use of one or more organic solvents. Also provided in part are compositions of polycarboxylic acids.
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Paragraph 0063-0064
(2015/12/30)
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- INTRAMOLECULAR END-TO-END REACTIONS OF PHOTOACTIVE TERMINAL GROUPS LINKED BY POLYMETHYLENE CHAINS.
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Intramolecular end-to-end reactions of a pair of photoactive terminal groups, dibenz left bracket b,f right bracket azepine (DBA) chromophores, linked by a series of polymethylene chains (DBA-CO(CH//2)//nCO-DBA, n equals 2-30) were studied by two different approaches. One approach is to measure the intramolecular deactivation rate constants of the excited triplet state of terminal DBA groups by the nanosecond laser photolysis and the other is to measure the intramolecular photocyclization rates of these bichromophoric compounds by the quantitative product analysis with GPC. The excited triplet state of the DBA group is the intermediate of the reaction.
- Ashikaga,Ito,Yamamoto,Nishijima
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p. 198 - 204
(2007/10/02)
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- One-step Synthesis of Long-chain Aliphatic α,ω-Dicarboxylic Acids Utilizing the Copper-catalyzed Reaction of β-Propiolactone with α,ω-Di-Grignard Reagents
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Copper-catalyzed reaction of β-propiolactone with α,ω-di-Grignard reagents, followed by esterification gave six-carbon homologated α,ω-dicarboxylic acid esters in good yields.
- Fujisawa, Tamotsu,Sato, Toshio,Kawara, Tatsuo,Tago, Hideyuki
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p. 345 - 346
(2007/10/02)
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