- Synthesis method of 4,4'-diphenyl ether dicarboxylic acid
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The invention discloses a 4,4'-diphenyl ether dicarboxylic acid synthesis method, which comprises: S1, carrying out a dehydration reaction on p-hydroxybenzoate, an alkali and a solvent at a temperature of 110-120 DEG C for 2-4 h under a protection gas to obtain a mixed solution; S2, adding a catalyst and p-halo benzoate into the mixed solution obtained in the step S1, carrying out a heating coupling reaction at a reaction temperature of 145-195 DEG C, adding a solvent after the reaction is finished, and performing extraction, liquid separation and crystallization to obtain a solid 4,4'-diphenyl ether dicarboxylic acid diester; and S3, carrying out heating hydrolyzing on the 4,4'-diphenyl ether dicarboxylic acid diester obtained in the step S2 in an aqueous alkali solution and a solvent, adding an acid to adjust the pH value to be acidic, and carrying out crystallization and filtration to obtain the 4,4'-diphenyl ether dicarboxylic acid. The method is simple in process operation, low inequipment requirement, high in product purity, less in three wastes generated in the production process, environment-friendly and high in industrial feasibility, and the total yield of the two-step reaction can reach more than 80%.
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Paragraph 0044; 0048-0049
(2020/05/01)
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- Method 4,4 ’ - for preparing diphenyl ether diformic acid
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The invention relates to preparation of a polymer monomer and especially relates to a preparation method of 4,4'-oxybisbenzoic acid. The preparation method comprises that 4-chlorobenzoic acid, 4-hydroxybenzoic acid and an acid binding agent are added into a polar high-boiling point solvent, the mixture undergoes a condensation reaction at a temperature of 140-280 DEG C until 4-chlorobenzoic acid content of the reaction system is in a range of 0.1-0.5%, and the polar solvent in the reaction system is diluted by water until the polar solvent has a mass concentration of 20-60% so that 4,4'-oxybisbenzoic acid is precipitated. The preparation method adopts easily available raw materials, has simple processes and mild reaction conditions, can be carried out under normal pressure, and has a low preparation cost, a high yield and high quality.
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Paragraph 0020-0033
(2019/11/17)
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- Method for preparation of 4, 4'-oxybisbenzoic acid by catalytic oxidation of Anderson type polyacid
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The invention discloses a method for preparation of 4, 4'-oxybisbenzoic acid by catalytic oxidation of Anderson type polyacid. The specific steps include: 1) subjecting di-p-tolyl ether, a heteropolyacid catalyst, an oxidant and an additive to oxidation reaction in a solvent; 2) at the end of the oxidation reaction, filtering out the heteropolyacid catalyst, and performing extraction to obtain anorganic phase and an aqueous phase; and 3) carrying out drying, filtering, concentration and purification on the organic phase in order to obtain 4, 4'-oxybisbenzoic acid, wherein the heteropolyacid catalyst is an Anderson polyacid parent or Anderson polyacid modified parent. The method provided by the invention adopts Anderson polyacid as the catalyst, which has the characteristics of high reaction activity, mild reaction conditions, environmental friendliness, high specificity and selectivity, recyclability, and is suitable for industrial production. Hydrogen peroxide, air or oxygen is adopted as the oxidant, can lower the cost, and also can reduce the emissions of three wastes and alleviate environmental protection pressure.
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Paragraph 0034; 0036; 0038; 0040; 0042
(2018/09/20)
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- Method for preparing 4,4'-oxybisbenzoic acid by using metal oxide to catalyze and oxidize
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The invention discloses a method for preparing 4,4'-oxybisbenzoic acid by using metal oxide to catalyze and oxidize. The method comprises the following steps of enabling dimethylphenyl ether to generate oxidizing reaction for 5 to 24h under the actions of an oxidant, an organic metal catalyst, a ligand and an additive at the oxidizing reaction temperature of 85 to 145 DEG C and the reaction gaugepressure of 1.0 to 5.0MPa; after the reaction is finished, treating, so as to obtain the 4,4'-oxybisbenzoic acid, wherein the organic metal catalyst is selected from one or two of cobalt acetate, manganese acetate, cerium acetate, cobalt nitrate, manganese nitrate, cobalt acetylacetonate, iron acetylacetonate or ceric ammonium nitrate; the additive is an alkaline substance. The method has the advantage that the metal oxides are used as the catalysts, and hydrogen peroxide, air or oxygen is used as the oxidant, so that the production cost is reduced, the generation of three wastes is reduced, the stress to environment is relieved, and the control and industrialized production are easy.
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Paragraph 0024-0029
(2018/07/30)
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- Facile aerobic photooxidation of methyl group in the aromatic nucleus in the presence of an organocatalyst under VIS irradiation
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We report a useful method for a facile synthesis of carboxylic acids from methyl aromatics by aerobic photooxidation using VIS irradiation and easily handled 2-chloroanthraquinone as organic catalysts under mild conditions such as an air atmosphere and ambient pressure and temperature. This is a more environmentally benign oxidation than previous methods, which require drastic reaction conditions.
- Tada, Norihiro,Hattori, Kasumi,Nobuta, Tomoya,Miura, Tsuyoshi,Itoh, Akichika
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supporting information; experimental part
p. 1669 - 1671
(2011/08/10)
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- Synthesis of aromatic carboxylic acids by carbonylation of aryl halides in the presence of epoxide-modified cobalt carbonyls as catalysts
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A new procedure was developed for synthesis of aromatic and heteroaromatic acids and their derivatives (esters, salts) by carbonylation of the corresponding aryl halides. The acids are selectively formed in a high yield under very mild conditions. Highly active catalytic systems, base-containing alcoholic solutions of cobalt carbonyl modified with epoxides, were used to activate aryl halides. 2005 Pleiades Publishing, Inc.
- Boyarskii,Zhesko,Lanina
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p. 1844 - 1848
(2007/10/03)
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- Correlation between molecular dipole moment and centrosymmetry in some crystalline diphenyl ethers
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The presence of a large molecular dipole moment in diphenyl ethers leads unequivocally to a centrosymmetric crystal structure. The Royal Society of Chemistry 2005.
- Dey, Archan,Desiraju, Gautam R.
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p. 2486 - 2488
(2007/10/03)
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- Preparation process of 4,4'-Dicarboxydiphenyl ethers or derivatives thereof
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4,4'-Dicarboxydiphenyl ether can be prepared by reacting diphenyl ether with an acetylating agent in the presence of a transition metal salt of trifluoromethane-sulfonic acid and an alkali metal perhalogenate to obtain 4,4'-diacetyldiphenyl ether and oxidizing the 4,4'-diacetyldiphenyl ether with an alkali metal hypohalogenite. A 4,4'-dicarboxydiphenyl ether, which is represented by the following formula (2): wherein Zs each represents -OH, -OR, -NH2, -NHR or -NR2, each R being an alkyl group having a carbon number not greater than 4, or a derivative thereof can be prepared by reacting a 4,4'-dihalodiphenyl ether, which is represented by the following formula (1): wherein X represents a halogen element, with carbon monoxide, a base and a nucleophile in the presence of a palladium catalyst and a bidentate phosphine compound.
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- Process for introducing a carboxyl group to an aromatic carboxylic acid or a derivative thereof
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Disclosed is a process for introducing a carboxyl group to an aromatic carboxylic acid or a derivative thereof, which comprises reacting a starting aromatic carboxylic acid, such as a benzoic acid, a biphenylcarboxylic acid, a naphthalenecarboxylic acid, a diphenylcarboxylic acid, or a derivative thereof, with a carbon tetrahalide in the presence of a cyclodextrin and an alkali metal hydroxide, thereby introducing a carboxyl group to the aromatic ring of the starting aromatic carboxylic acid or the derivative thereof in substitution for a hydrogen atom bonded thereto. By the process of the present invention, a desired aromatic polycarboxylic acid or a derivative thereof can be easily obtained with high selectivity.
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