【摘要】 为控制盐酸度洛西汀的质量,本研究以2-噻吩甲醛和膦酰基乙酸三乙酯为原料,经Horner-Wadsworth-Emmons反应、DIBAL-H还原、氧化、Friedel-Crafts反应、甲胺/硼氢化钠还原胺化制得欧洲药典7.5版收载的2-[3-甲胺基-1-(2-噻吩基)丙基]-1-萘酚(有关物质E),并经1H NMR、13C NMR和HRMS确证结构。更多还原

【Abstract】 To perform the quality control of duloxetine hydrochloride, the related substance 2-[3-(methylamino)-1-(thiophen-2-yl)propyl]naphthalen-1-ol(related substance E) recorded in EP 7.5 was prepared from 2-thenaldehyde and triethyl phosphonoacetate via Horner-Wadsworth-Emmons reaction, reduction with diisobutyl aluminium hydride, oxidation, Friedel-Crafts reaction and reductive amination with methylamine/sodium borohydride. The structure was confirmed by 1H NMR, 13 C NMR and HRMS.更多还原