1217-67-0Relevant academic research and scientific papers
Process for the Preparation of Ethacrynic Acid
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Paragraph 0077, (2018/05/03)
The invention provides an improved process for preparing Ethacrynic acid of formula I, including the steps of: (a) reacting 4-butyryl-2,3-dichloro-phenoxy acetic acid of formula II with dimethylamine or its salt to obtain [2,3-dichloro-4-[2-dimethylaminomethyl butyryl phenoxy acetic acid of formula III or its salt; (b) hydrolysing [2,3-dichloro-4-[2-dimethylaminomethyl butyryl phenoxy acetic acid hydrochloride of formula III obtained in step a) with t-butyl amine to obtain t-butyl amine salt of Ethacrynic acid; (c) acidifying the t-butyl amine salt of Ethacrynic acid formed in step b) to obtain Ethacrynic acid of formula I; and(d) optionally purifying the obtained Ethacrynic acid with a solvent mixture of alkyl acetate and hydrocarbon solvent. The invention also provides crystalline t-butylamine salt of Ethacrynic acid and process thereof. Also provide compound Ethacrynic acid having a purity of greater than or equal to 99% and a composition including the compound.
Environmental-protection preparation method for high yielding of 1,2,4-oxadiazole compounds containing alpha,beta-unsaturated ketones
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Paragraph 0069; 0070; 0071, (2017/08/30)
The invention provides an environmental-protection preparation method for high yielding of 1,2,4-oxadiazole compounds containing alpha,beta-unsaturated ketones; with 2,3-dichlorophenol as a raw material, an intermediate 5 is obtained through methylation and protection of phenolic hydroxyl groups, Friedel-Crafts acylation, methyl protecting group removal, nucleophilic substitution, ester hydrolysis, aldol condensation and dehydration reaction and then undergoes cyclization reaction with substituted amine oxime to obtain the target products 6r, 6s and 6u. The method has the advantages of mild reaction conditions, has no use of first-class reagents and other reagents harmful on the environment and operating personnel, fewer by-products, stable and controllable reactions, simple postprocessing, high yield and purity, and easy industrialized production.
Liquid chromatographic analysis of ethacrynic acid and degradation products in pharmaceutical systems
Yarwood,Moore,Collett
, p. 220 - 223 (2007/10/02)
An accurate, reproducible, and specific reversed-phase high-performance liquid chromatographic (HPLC) system was developed for the determination of ethacrynic acid and its degradation products. The method was used in stability studies of the drug in the solid state, in solution, and in dosage forms. Three degradation products were isolated by preparative chromatography and identified by several techniques, principally NMR and MS. TLC R(f) and HPLC response factors are quoted. A degradation scheme consistent with the observed stability profiles is proposed.
