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以乙酰基二茂铁为原料,经过钯催化氢化胺化及(R)-(+)-酒石酸拆分制备了(R)-1-二茂铁基乙基二甲胺(Ⅲ);Ⅲ与正丁基锂作用后,与二苯基氯化膦作用得到N,N-二甲基-(R)-1-[(S)-2-(二苯基膦)二茂铁基]乙胺(Ⅳ);Ⅳ与新制的二(3,5-二甲基苯基)膦烷发生构型保持的取代反应,得到双膦配体(R)-1-[(S)-2-(二苯基膦)二茂铁基]乙基二(3,5-二甲基苯基)膦(Ⅷ)。以乙酰基二茂铁计Ⅷ的总收率达19.5%,手性高效液相色谱分析其ee值达95%。
(R) -1-ferrocenyl ethyl dimethylamine (Ⅲ) was prepared from acetylferrocene via palladium-catalyzed hydrogenation and (R) - (+ After the action of n-butyllithium and diphenylphosphine chloride, N, N-dimethyl- (R) -1 - [(S) -2- (diphenylphosphino) ferrocenyl] ethylamine (Ⅳ) Ⅳ. The substitution reaction of Ⅳ with the new configuration of bis (3,5-dimethylphenyl) phosphorane gives the bisphosphine ligand (R) -1 - [(S) -2- Phenylphosphino) ferrocenyl] ethylbis (3,5-dimethylphenyl) phosphine (VIII). The total yield of Ⅷ with acetyl ferrocene was 19.5%, and its ee was 95% by chiral high performance liquid chromatography.