摘要
Aim To determine the structure of the by-product produced in Grignard reaction for preparing mifepristone derivatives, and elucidate the reaction mechanism.Methods The structure of the by-product was determined with elemental analysis, one- and two-dimension spectra NMR (DEPT, 1H-1Hcosy, HMQC, HMBC) and compared with those of mifepristone.Results The main by-product was 11,17-di-addition product of Grignard reagent of N, N-dimethylamino phenyl bromide.Conclusion This is the first complete assignment of 1H NMR and 13C NMR of compound (3).
目的 确定米非司酮衍生物制备过程中格氏反应一步的副产物的结构 ,并分析反应机理。方法 通过一维及二维光谱分析和元素分析确定副产物的结构。结果 证实了副产物是 11,17位双加成的格氏反应的产物。结论 这是首次对此步副产物用光谱进行C ,H的详细归属。
