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本文以三苯甲基保护的厄贝沙坦为起始原料,经酸去保护得到厄贝沙坦盐酸盐,然后以碳酸氢钠为滴定剂,在乙醇和水的混和溶媒中,调节结晶体系达到一定的pH值析晶,从而得到单一晶型的厄贝沙坦晶型B产物。厄贝沙坦晶型B通过X-单晶衍射仪检测法,同时与厄贝沙坦晶型A和已报道厄贝沙坦晶型B的文献对比确证。我们提出了一种新的厄贝沙坦晶型B的合成工艺,简化了制备晶型B的步骤。
In this paper, trityl-protected irbesartan as a starting material, by acid deprotection to obtain irbesartan hydrochloride, and then sodium bicarbonate as titrant in a mixed solvent of ethanol and water to adjust the crystallization The system reaches a certain pH value of crystallization, so as to obtain a single crystal form of irbesartan B product. Irbesartan Form B is confirmed by X-ray single crystal diffractometry and is contrasted with the literature of Irbesartan Form A and reported Irbesartan Form B. We propose a new synthesis of irbesartan crystalline form B, simplifying the preparation of Form B step.