| 摘要 |
PURPOSE: A manufacturing method of amlodipine besylate of formula (1) is provided which simplifies existing process by synthesizing amlodipine besylate directly from a novel triazone compound of formula (5) in high yield of more than 90%. CONSTITUTION: A preparation method of amlodipine besylate(2-£(2-(1,3-dimethylhexahydro-2-oxo-1,3,5-triazine-5-yl)ethoxy)-methyl|-4-(2-chlorophenyl)-3- ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine) comprises the steps of: dissolving 5g(17mmol) of ethyl 4-£1,3-dimethylhexahydro-2-oxo-1,3,5-triazine-5-yl|acetoacetate in 50ml of isopropanol(or acoholic solvent like as methanol, ethanol); adding 2.33g of 2-chlorobenzaldehyde and circulating for 1hr; cooling to room temperature, adding small quantity of acetic acid to neutralize; adding 1.97g of methyl 3-aminochlotonate to the solution, and circulating for 18hrs; concentrating under decompression to get brown oily residue; performing silicagel column chromatography to get 4.5g of objective material.
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