- Preparation method of lodoxamide tromethamine intermediate
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The invention belongs to the technical field of medicine chemical engineering, and particularly discloses a preparation method of a lodoxamide tromethamine intermediate of lodoxamide. The method comprises the following steps of (1) dissolving 3,5-diamino-4-chlorobenzonitrile into an organic solvent to form a solution A; (2) dissolving oxalyl chloride into the organic solvent to form a solution B;(3) slowly dripping the solution A into the solution B; in the dripping process, controlling the temperature of the reaction liquid at -20 to 0 DEG C; after the reaction is completed, slowly drippinga certain amount of ice water into the reaction liquid; after the dripping is completed, continuously performing stirring for 0.5 to 1h; then, performing suction filtering; drying obtained filter caketo obtain lodoxamide. The reaction steps of the method are few; the operation is facilitated; the yield is greatly improved and can reach 90 percent or higher; meanwhile, the related impurities of the product lodoxamide are few; the product purity is high; the HPLC purity can reach 99.5 percent or higher; great significance is realized on the synthesis of the lodoxamide tromethamine medicine.
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Paragraph 0048; 0049
(2018/12/13)
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