16523-31-2Relevant articles and documents
A Safe Cost-Efficient Synthesis of 4,6-Diaminoresorcinol
Pews, R. Garth,Lysrnko, Zenon,Vosejpka, Paul C.
, p. 8255 - 8256 (1997)
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Benzo [1,2-d:5,4-d '] b (oxazole) - 2,6-di-thiol and its preparation method
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Paragraph 0013; 0024-0026, (2018/09/02)
The invention discloses benzo [1, 2-d: 5, 4-d']-di-(oxazole)-2, 6-dithiol and a preparation method thereof. The preparation method comprises the steps as follows: resorcinol is taken as a raw material, zinc chloride is taken as a catalyst, resorcinol and zinc chloride react with acetic oxide to obtain 4, 6-diacetylresorcinol; 4, 6-diacetylresorcinol reacts with hydroxylamine hydrochloride in sodium hydroxide to obtain 4, 6-di-[(1Z)-N-hydroxyethyliminumacyl]benzene-1, 3-diphenol; 4, 6-di-[(1Z)-N-hydroxyethyliminumacyl]benzene-1, 3-diphenol is taken as a raw material and subjected to Beckmann rearrangement reaction in a polyphosphoric acid system to obtain DAR*HCl; and DAR*HCl is taken as a raw material and reacts with carbon disulfide in a potassium hydroxide solution to obtain a target compound. According to the invention, sulfydryl is introduced at 2 and 6 sites simultaneously, the product is prepared through multiple steps of reaction, the method is simple, convenient and easy to operate, the melting point of the product is higher than 300 DEG C, and the yield is high.
One-pot synthesis preparation 4,6-diaminoresorcinol method of hydrochloride
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, (2016/10/08)
The invention discloses a method for preparing 4,6-diaminoresorcinol dihydrochloride through one-pot synthesis. The method mainly comprises the steps of: by taking Bronsted acid such as polyphosphoric acid, concentrated sulfuric acid or methanesulfonic acid as the catalyst and the solvent, realizing oximation, Beckmann rearrangement, hydrolysis and hydrocchlorination of 4,6-diacetylresorcinol, and thus obtaining the 4,6-diaminoresorcinol dihydrochloride (DAR.2HCl), wherein the mol ratio of hydroxylamine hydrochloride, the Bronsted acid catalyst and the 4,6-diacetylresorcinol is (2.0-2.5)/(1-10)/1, and the reaction temperature ranges from 65 to 125 DEG C. The method provided by the invention is simple in process steps and efficient in preparation; therefore, the industrialization of the 4,6-diaminoresorcinol dihydrochloride is greatly promoted.