254-82-0Relevant articles and documents
Synthesis method of dipyridamole intermediate
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Paragraph 0027; 0028; 0030; 0031, (2018/06/04)
The invention relates to the technical field of medicine and material intermediates, in particular to a synthesis method of a dipyridamole intermediate. The method is characterized in that pyrimido-[5,4-D]pyrimidine crude products are added into a solvent A; then, a bromination reagent is added; temperature rise is performed till the backflow; reaction is performed for 24 to 48h; after HPLC (HighPerformance Liquid Chromatography) detection display raw materials disappear, reaction stops; aftertreatment and drying are performed to obtain tetrabromo pyrimido-[5,4-D]pyrimidine crude products; (2) the tetrabromo pyrimido-[5,4-D]pyrimidine crude products obtained in the step (1) are added into concentrated hydrochloric acid; heating is performed till the backflow; backflow reaction is maintained for 24 to 36h; the reaction is completed; the temperature is lowered to the room temperature after the reaction stops; aftertreatment and drying are performed to obtain a crude product; after the crude product is recrystallized, drying is performed to obtain the product. The synthesis method has the beneficial effects that the experiment steps are reduced; nitratlon reaction with higher risk and the use of phosphorus pentachloride/phosphorus oxychloride with high toxicity are avoided; the product purity is greater than 98 percent; the total yield is higher than 50 percent; the operation issimple and convenient; the number of three wastes is greatly reduced; the use of strong corrosion and risk reagents is avoided; the safety coefficient is high; the synthesis method is applicable to industrial production.
