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.
Preparation process of anti-infective drug nifuratel
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Paragraph 0024; 0051-0056, (2018/05/16)
The invention belongs to the technical field of drug synthesis and in particular relates to a preparation process of an anti-infective drug nifuratel. The preparation process comprises the following steps: taking iodomethane, sodium sulfide and chlorocyclopropane as initial raw materials to obtain epoxy propyl methyl sulfide, carrying out ring-opening reaction with hydrazine hydrate to obtain 3-methylmercapto-2-hydroxyl-propylhydrazine, carrying out a ring-closure reaction to obtain N-amino-5-methylthiomethyl-2-oxazolidinone, hydrolyzing 5-nitro furfural diacetate in the presence of trifluoroacetic acid to obtain 5-nitro-2-furancarboxaldehyde, and performing condensation with N-amino-5-methylthiomethyl-2-oxazolidinone, thereby obtaining the nifuratel. Safe and cheap reagents are selected in the process route, and environment hazards are reduced. Meanwhile, the operating difficulty and reaction after-treatment burdens are reduced, the production safety is ensured, the process is a simple, green and economic process route for preparing the nifuratel, and the obtained product is high in yield, excellent in purity and suitable for large-scale industrial production of the nifuratel.
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.