- Continuous flow synthesis method of 2-(2-aminothiazole-4-yl)-2-methoxyiminoacetic acid intermediate
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The invention discloses a continuous flow synthesis method of an 2-(2-aminothiazole-4-yl)-2-methoxyiminoacetic acid intermediate, and belongs to the technical field of organic synthesis. The method comprises the following steps: (1) enabling 2-methoxyimino ethyl acetoacetate to pass through a material channel A of a continuous flow microreactor, enabling sulfonyl chloride to pass through a material channel B, enabling a catalyst and an initiator to pass through a material channel C and respectively flow into a reaction channel with a preset temperature through metering pumps P1, P2 and P3 formixing reaction, and enabling reaction liquid to flow out from a discharge port after the reaction is finished; and (2) after the reaction liquid flows out, dropwise adding the reaction liquid into athiourea aqueous solution, controlling the pH value to react, adjusting the pH value to be neutral after the reaction is finished, cooling, filtering, washing and drying to obtain the 2-(2-aminothiazole-4-yl)-2-methoxyiminoacetic acid. By using the continuous flow microreactor, the continuous reaction is realized, the process is stable and easy to control, the reaction toxicity is low, the yield can reach 92.94%, and the product purity can reach 99.55%.
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Paragraph 0030-0035
(2021/03/11)
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- Synthetic method for ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate
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The invention discloses a synthetic method for ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate. The method is characterized by comprising the following steps: a, performing chlorination on diketene, and performing alcoholysis to synthesize ethyl 4-chloroacetoacetate; b, performing oximation on the ethyl 4-chloroacetoacetate to synthesize ethyl 4-chloro-2-(hydroxyimino)-3-oxobutanoate; c, performing a reaction on the ethyl 4-chloro-2-(hydroxyimino)-3-oxobutanoate and thiourea to synthesize ethyl 2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetate; and d, performing hydrocarbonylation on the ethyl2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetate to synthesize the ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate. The method has the following advantages: 1, the chlorination reaction in the stepa is a continuous reaction, and has a fast reaction speed and no accumulation of a large amount of dangerous materials, so that the danger is small; 2, the costs of equipment are lower, the equipmentis conventional organic synthesis equipment, no expensive and special equipment is needed, so that the equipment is easy to copy, and the production efficiency is improved; and 3, the diketene is directly used as a raw material, the raw material cost is low, the synthetic steps are simple to operate, so that the method facilitates reducing the production costs of the ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate.
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- The jig measuring method for measuring the shape of the film surface,
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PROBLEM TO BE SOLVED: To provide a fixing tool for measuring a film surface shape and a method of measuring the film surface shape for suppressing the influence of a film fixing method and the like on the measurement data to the minimum, when quantitatively measuring film surface shape. SOLUTION: The fixing tool for measuring film surface shape, being the film fixing tool used when measuring the shape of film surface or the shape of a structure formed on the film surface has: a mechanism for holding the circumference of the measuring area of the film surface from both top and bottom directions of the film; and a mechanism for pulling it in both outward directions of the XY plane of the film. Preferably, the mechanism for holding the film from both top and bottom directions of the film is so constituted that a fixing tool made of parallel flat plates holds the film from both the top and bottom. COPYRIGHT: (C)2010,JPOandINPIT
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- Pseudosaccharin amine derivatives: Synthesis and elastase inhibitory activity
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Pseudosaccharin amines were synthesized from saccharin either by the reaction of pseudosaccharin chloride with amines, or via thiosaccharin which was treated with amines yielding thiosaccharinates, and their reaction with glacial acetic acid. This route gave lower yields than the first way. The synthesis of alkyl [(1,1-dioxo-benzo[d]isothiazol-3-yl)amino]alkanoates as possible Human Leukocyte Elastase (HLE) inhibitors was realized by the reaction between amino acid esters and pseudosaccharin chloride. Hydrolysis of the esters was possible under aqueous basic conditions. Selected compounds were screened for elastase inhibitory activity. Compounds 4k and 4m were found to be reversible inhibitors of HLE with Ki values of 45 μM and 60 μM.
- Rode, Haridas B.,Sprang,Besch,Loose,Otto, Hans-Hartwig
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p. 723 - 731
(2007/10/03)
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