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目的合成异环磷酰胺原料药中的一种有关物质。方法以3-氨基丙醇为原料,与三氯氧磷环合制得2-氯-1-氧杂-3-氮杂-2-磷杂环己烷-2-氧化物(3);以1-氨基-2-丙醇为原料,与氯化亚砜反应制得2-氯丙胺盐酸盐(5);化合物3与5经取代、酰化、还原得到有关物质3-(2-氯乙基)-2-[(2-氯丙基)氨基]-1-氧杂-3-氮杂-2-磷杂环己烷-2-氧化物。结果与结论合成了异环磷酰胺原料药中的一种有关物质,其结构经1H-NM R、13C-NM R和M S谱确证,纯度在99%以上。该有关物质可作为异环磷酰胺原料药质量控制的对照品。
Objective To synthesize a related substance in ifosfamide raw material medicine. Methods 3-Aminopropanol was used as a starting material to cyclize with phosphorus oxychloride to prepare 2-chloro-1-oxa-3-aza-2-phosphacyclohexane-2-oxide (3) 2-chloro-propylamine hydrochloride (5) was prepared by the reaction of 1-amino-2-propanol and thionyl chloride. The compounds 3 and 5 were substituted, acylated and reduced to obtain 3- Ethyl) -2 - [(2-chloropropyl) amino] -1-oxa-3-aza-2-phospyclohexane-2-oxide. RESULTS AND CONCLUSIONS A related substance of ifosfamide was synthesized and its structure was confirmed by 1H-NM R, 13C-NM R and M S spectra with a purity of over 99%. The related substances can be used as ifosfamide raw material quality control reference substance.