- Synthesis method of diclofenac sodium
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The invention discloses a synthesis method of diclofenac sodium, which comprises the following steps: (1) toluene. An oil layer is obtained by adding 2, 6 -dichlorophenol and sodium carbonate, keeping warm and refluxing, extracting the oil layer with water, and adding an alkali heat-preserving reaction in the oil layer to obtain 2, 6 -dichloroaniline. (2) 1, 2 Dichlorodimethylaniline prepared in step (6 -) is heated and melted, chloroacetyl chloride is added dropwise, and the heat is subjected to heat preservation reaction after being heated to crystallize to obtain N - (2, 6 - dichlorophenyl) - phenyl - chloroacetamide. (3) 2 (N - 2 Dichlorophenyl) 6 - phenyl - chloroacetamide prepared in step (-) is reacted with the aluminum trichloride to give a solid 1 - (2, 6 -dichlorophenyl) -2 -indolinone. (4) 3 (1 - 2-dichlorophenyl) 6 -indolinone prepared in step (-2 -) is added to alkali liquor, stirred and heated to reflux to obtain diclofenac sodium. The synthesis method is stable, easy to operate, low in cost, high in yield and suitable for industrial production.
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Paragraph 0024; 0028; 0032
(2021/09/21)
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- MATERIALS FOR ORGANIC ELECTROLUMINESCENT DEVICES
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The present invention relates to compounds suitable for use in electronic devices, and to electronic devices, especially organic electroluminescent devices, comprising these compounds.
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Paragraph 0084-0085
(2021/02/23)
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- Preparation method of 2, 6-dichlorodiphenylamine
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The invention belongs to the technical field of chemical drug synthesis and specifically relates to a preparation method of 2, 6-dichlorodiphenylamine. The preparation method of the 2, 6-dichlorodiphenylamine comprises the following steps: (1) adding 2, 6-dichlorodiphenylamine and a polar aprotic solvent into a reaction bottle; after the 6-dichlorodiphenylamine and the polar aprotic solvent are stirred and dissolved, adding chlorobenzene, alkali and a catalyst to an obtained mixture; stirring and heating the mixture to 120-160 degrees centigrade; and preserving the heat of the mixture for reaction for 2-4 h, wherein the catalyst is nanometer copper oxide or nanometer copper iodide; and (2) cooling a reaction mixture obtained in the step (1) to 50-90 degrees centigrade; filtering the cooledreaction mixture; carrying out reduced pressure distillation on a filter liquor to obtain a crude product; and purifying the crude product to obtain the 2, 6-dichlorodiphenylamine. The preparation method of the 2, 6-dichlorodiphenylamine, provided by the invention, has the advantages that the catalytic efficiency of the catalyst is high, the usage of the catalyst is less, the selectivity of a reaction solvent is good, the reaction solvent is easy to recover, the raw material cost is low, the yield of a prepared product is high, the purity is high, the quality is high, and the preparation method of the 2, 6-dichlorodiphenylamine is easy to realize industrial production and application.
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Paragraph 0025-0038; 0042-0069; 0073-0088; 0092-0111
(2019/09/05)
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- A synthetic method for diclofenac zinc
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The invention relates to a synthetic method for diclofenac zinc, and belongs to the field of chemical synthesis of medicines. Aniline is adopted as a raw material and is reacted with 2,6-dichlorophenol under the action of acetyl chloride to obtain 2-(2,6-dichlorophenoxy)-N-phenylacetamide; the 2-(2,6-dichlorophenoxy)-N-phenylacetamide is adopted to prepare N-(2,6-dichlorophenyl)phenylamine under action of an inorganic alkali; the N-(2,6-dichlorophenyl)phenylamine is subjected to a cyclization reaction under the action of chloroacetyl chloride to prepare 1-(2,6-dichlorophenyl)-2-indolone; and the 1-(2,6-dichlorophenyl)-2-indolone is subjected to hydrolysis, and other reactions to synthesize the diclofenac zinc. According to the method, the cost is low, the yield is high, the total yield is 70%, reaction conditions are mild particularly, the method is environment-friendly, and waste gas generated in a reaction process, such as hydrogen chloride, is absorbed by an absorbing system, and therefore the method has a good industrialization prospect.
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- Simultaneous identification of Fenton degradation by-products of diclofenac, ibuprofen and ketoprofen in aquatic media by comprehensive two-dimensional gas chromatography coupled with mass spectrometry
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Diclofenac, ibuprofen and ketoprofen are anti-inflammatory drugs intensively used both in human and animal treatment. Due to their high stability these compounds are partially removed by wastewater treatment plants and from this reason the development of some alternative treatments such as advanced oxidative processes are necessary. The main problems in the optimization of an advanced oxidative process rise from the difficulties which appear in the identification of degradation by-products necessary for the establishment of degradation pathway. In this paper a developed method for the simultaneous identification of Fenton degradation by-products of the three above mentioned pharmaceuticals is presented. The obtained results show the comprehensive two-dimensional gas chromatography coupled with mass spectrometry as a proper method for the analysis of the complex mixture of compounds resulted from the Fenton degradation process. Moreover, some compounds never mentioned in the scientific literature were identified. (Chemical Equation Presented).
- Beldean-Galea, Mihail Simion,Coman, Virginia,Copaciu, Florina,Thiébaut, Didier,Vial, Jér?me
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p. 1021 - 1027
(2015/07/15)
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- Direct amination of phenols under metal-free conditions
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Herein, we disclose the metal-free synthesis of arylamines via the direct amination of phenols using aminating reagents. This reaction procedure uses easy accessible aminating reagents and provides a versatile synthetic route to a broad range of arylamines with various functionalities in good to excellent yield. By using a two-step route of amination and oxidative coupling reaction, we synthesized three naturally occurring carbazole alkaloids: murrayafoline A, mukonine, and clausenine from two commercially available phenols. Georg Thieme Verlag Stuttgart · New York.
- Yu, Jianzhong,Wang, Yongtao,Zhang, Peizhi,Wu, Jun
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supporting information
p. 1448 - 1454
(2013/07/26)
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- Industrial-scale palladium-catalyzed coupling of aryl halides and amines - A personal account
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The palladium-catalyzed coupling of amines and aryl halides or aryl alcohol derivatives has matured from an exotic small-scale transformation into a very general, efficient and robust reaction during the last ten years. This article reports several applications of this method from an industrial vantage point, including ligand synthesis, synthesis of arylpiperazines, arylhydrazines and diarylamines. Much emphasis in placed on issues of scale-up and safety to underline the potential of C-N couplings as solutions for industrial-scale synthetic problems.
- Buchwald, Stephen L.,Mauger, Christelle,Mignani, Gerard,Scholz, Ulrich
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- Method for the preparation of substituted derivatives of diphenyl amine
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This invention provides a novel process for the preparation of substituted derivatives of diphenyl amine. The special feature of this novel process is that low cost and recoverable phenolic salts are used as catalysts for molecular rearrangement and aminolysis to obtain substituted derivatives of diphenyl amine in high yield.
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- N-phenyl-2,2,6,6-tetrahalocyclohexaneimine
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A process for preparing a 2,2,6,6-tetrahalocyclohexanimine derivative (I) which comprises reacting a 2,2,6,6-tetrahalocyclohexanone with a primary amine or ammonia in the presence of a Lewis acid, a process for preparing a 2,6-dihaloaniline derivative (II) which comprises subjecting the 2,2,6,6-tetrahalocyclohexaneimine derivative (I) to dehydrohalogenation in the presence or absence of a catalyst, and an N-phenyl-2,2,6,6-tetrahalocyclohexaneimine. According to the process of the present invention, the 2,2,6,6-tetrahalocyclohexaneimine derivative (I) can be prepared from inexpensive starting materials in high yield through a few steps. Also, the 2,6-dihaloaniline derivative (II) can be prepared from inexpensive starting materials in high yield and high purity through a few steps. Further, the N-phenyl-2,2,6,6-tetrahalocyclohexaneimine is very useful in the preparation of N-phenyl-2,6-dihaloaniline.
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- Process for the preparation of 2,6-dichlorodiphenylaminoacetic acid derivatives
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A new process for the preparation of 2,6-dichlorodiphenylamine derivatives is described, which process provides the desired active compound in a high yield and with a very high degree of purity by a technically simple and realizable procedure.
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