34272-64-5Relevant academic research and scientific papers
Method for synthesizing cefodizime sodium intermediate 2-mercapto-4-methyl-5-thiazoleacetic acid
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Paragraph 0029-0043, (2018/04/21)
The invention relates to a method for synthesizing a pharmaceutical intermediate, in particular to a method for synthesizing a cefodizime sodium intermediate 2-mercapto-4-methyl-5-thiazoleacetic acid.The method comprises the following steps of adding ammonium dithiocarbamate into an alkaline solvent, raising the temperature, dropwise adding 3-chloropropanoate, and conducting heat-preservation stirring; adding activated carbon for decolorization after dissolved clarification, conducting filtering, and conducting decompression distillation on obtained filtrate; washing and filtering solid products after the distillation with water, and conducting vacuum drying on remaining solid products to obtain 2-mercapto-4-methyl-5-thiazoleacetic acid. By means of the method, the product yield is greater than or equal to 60%, the product purity is greater than or equal to 99.5%, the production rate is obviously increased, the production cost is reduced, and the method meets the needs of industrial production.
Synthesis method of 2-sulfydryl-4-methyl-5-thiazole acetic acid
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Paragraph 0024; 0025; 0026; 0027; 0028; 0029-0034, (2018/03/28)
The invention relates to a synthesis method of a 2-sulfydryl-4-methyl-5-thiazole acetic acid. The synthesis method comprises the following steps: adding a levulinic acid and an organic solvent into areaction kettle, adding a compound A, slowly adding a catalyst, stirring, raising the temperature to 40-60 DEG C, preserving the heat for 2-2.5 hours, adding water for washing, layering to obtain an organic phase, directly adding ammonium dithiocarbamate, water and a compound B into the organic phase to perform a ring-closure reaction, layering after finishing the reaction to obtain an aqueous phase, and regulating the pH of the aqueous phase to obtain the 2-sulfydryl-4-methyl-5-thiazole acetic acid. The synthesis method is simple in operation, high in yield, low in cost and short in operationcycle, and is easy to control. The heterogeneous reaction is realized, the procedure of distilling the organic solvent is reduced, the reaction procedure is reduced, and the production time is shortened. The power consumption is reduced. The loss of the organic solvent in the distilling process is reduced, and the environment pollution caused by the organic solvent is further reduced.
