45378-62-9Relevant articles and documents
Preparation method of nifuratel intermediate
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Paragraph 0029-0031; 0038-0040; 0048-0050; 0057-0059; 0066, (2021/05/01)
The invention provides a preparation method of a nifuratel intermediate. The preparation method comprises the following steps: (1) reacting sodium methyl mercaptide with epoxy chloropropane to prepare 2-(methylthio methyl)-oxetane; (2) dropwise adding 2-(methylthio methyl)-oxetane into hydrazine hydrate to prepare 3-methylthio-2-hydroxy-propyl hydrazine; (3) adding diethyl carbonate into 3-methylthio-2-hydroxy-propyl hydrazine to prepare a nifuratel intermediate, namely N-amino-5-methylthio methyl-2-oxazolidinone; and (4) salifying the prepared N-amino-5-methylthio methyl-2-oxazolidinone and concentrated hydrochloric acid to prepare the nifuratel intermediate hydrochloride. According to the preparation method of the nifuratel intermediate, disclosed by the invention, the nifuratel intermediate can be conveniently and quickly obtained, and the obtained nifuratel intermediate is high in yield, high in purity and stable in quality.
A synthetic method of Nifuratel (by machine translation)
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Paragraph 0022; 0024; 0025, (2018/11/22)
The invention discloses a method for synthesizing Nifuratel. The method of the invention is sodium methyl mercaptan, ech in catalyst-tetrabutyl ammonium bromide under the effect of the compound into a sulfur [...] propane, resulting a sulfur [...] propane and hydrazine reflux 1 - 3 hours to be hydrazinolysis, to obtain 3 - methylthio - 2 - hydroxy [...]; and the resulting reaction mixture in sodium methoxide under the action of the cyclization, shall be N - amino - 5 - methylthio methyl - 2 - oxazolidone, the resulting product with the 5 - nitro furfural b ethyl ester in dilute mineral acid conditions condensation, get the yellow powder 5 - [(methylthio) methyl] - 3 - [[ (5 - nitro - 2 - furyl methylene] amino] - 2 - oxazolidone. This invention lies in the use of its primary product with the raw material of the nature of the nature of the difference between the direct chemical combination, without rectification and purification, overcomes the tedious operation in production steps, simplifies the synthesis method, convenient for large-scale industrial production. (by machine translation)
Nifuratel method for the preparation of
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Paragraph 0045; 0046, (2016/12/01)
The invention relates to a method for preparing nifuratel. The method comprises the steps of (1) synthesizing 2-(methylmercapto-methyl)-oxacyclopropane through epoxy chloropropane and sodium methyl mercaptide; (2) generating reaction between hydrazine hydrate and the 2-(methylmercapto-methyl)-oxacyclopropane to synthesize 3-methylmercapto-2-hydroxy-propyl hydrazine; (3) generating reaction between diethyl carbonate and 3-methylmercapto-2-hydroxy-propyl hydrazine to prepare N-amino-5-methylmercapto-methyl-2-oxazolidinone; (4) hydrolyzing 5-nitrofuran formaldehyde diacetate ester under an acidic condition to prepare 5-nitro-2-furaldehyde; (5) generating reaction between the 5-nitro-2-furaldehyde and the N-amino-5-methylmercapto-methyl-2-oxazolidinone obtained in the step (3) to obtain the nifuratel, wherein in the step (1), 15-crown ether-5 is used as a catalyst, so that the conversion rate is high; no organic solvent is used during posttreatment of a product, and the posttreatment is simple.