知识与财富的链接
以L-天冬氨酸为原料,经缩合得N-甲酰-L-天冬氨酸酐,然后经酰化、酯化、还原、成环得(S)-1-苄基-3-氨基吡咯烷,最后脱苄合成(S)-(+)3-氨基吡咯烷二盐酸盐,总收率62.8%。考察了工艺条件对反应的影响。(S)-1-苄基-3-氨基吡咯烷适宜工艺条件为:n(KBH4)∶n(H2SO4)∶n(混合物4)=3∶1.5∶1,反应温度50～60℃,反应时间6h,收率71.6%。产物结构经MS和1 H NMR进行确证。
N-Formyl-L-aspartic anhydride was prepared via condensation reaction with L-aspartic acid,then the compound(S)-1-benzylpyrrolidin-3-amine was obtained from N-formyl-L-aspartic anhydride via acylation,esterification,reduction and ring closing,finally(S)(+)-3-Aminopyrrolidine dihydrochloride was obtained through debenzylation with the total yield of 62.8%.The effect of synthesis conditions on(S)-1-benzylpyrrolidin-3-amine was studied.The optimal reaction conditions were found as follows : the yield could reach 71.6% when n(KBH 4) ∶n(H 2 SO 4) ∶n(Compound 4) =3∶1.5∶1 and reacted 6hat 50-60℃.The target compound was confirmed by MS and 1 H NMR.
