- Synthesis method of irinotecan hydrochloride
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The invention discloses a synthesis method of irinotecan hydrochloride, belonging to the technical field of compound preparation. The synthesis method comprises the following steps: (1) in the presence of an organic solvent, alkali and a catalyst, subjecting 7-ethyl-10-hydroxycamptothecin to full reactionwith 4-piperidinyl piperidinecarbonyl chloride at room temperature, quenching the reaction by using a 5% sodium bicarbonate solution, and separating out an organic phase; and (2) adding normal hexane into the organic phase obtained in the step (1) for crystallization, performing filtering, adding an organic solvent and concentrated hydrochloric acid into a filter cake, conducting reacting to obtain a crude irinotecan hydrochloride product, and purifying the crude irinotecan hydrochloride product to obtain irinotecan hydrochloride. According to the invention, carbonate is used as a catalyst, charging is convenient, and generated products are carbon dioxide and water and are friendly to a system; and in addition, n-hexane is adopted as a reverse solvent for crystallization, yield is high, post-treatment is convenient, and industrial mass production is facilitated.
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Paragraph 0026-0028
(2021/07/17)
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- PREPARATION METHOD
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The present invention is directed to a novel method for the preparation of high purity irinotecan. This can be achieved by eliminating the excess of the other reagent, bipiperidinyl-1'-carbonyl chloride after it has reacted with 7-ethyl-10-hydroxy camptothecin and crystallizing the final product from a suitable solvent.
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Page/Page column 6
(2008/06/13)
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