15307-93-4Relevant articles and documents
Synthesis method of diclofenac sodium
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Paragraph 0024; 0028; 0032, (2021/09/21)
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.
Preparation method of 2, 6-dichlorodiphenylamine
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Paragraph 0025-0038; 0042-0069; 0073-0088; 0092-0111, (2019/09/05)
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.
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
Beldean-Galea, Mihail Simion,Coman, Virginia,Copaciu, Florina,Thiébaut, Didier,Vial, Jér?me
, p. 1021 - 1027 (2015/07/15)
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).