(S)-(+)3-氨基吡咯烷二盐酸盐的合成研究

SYNTHESIS OF (S)(+)-3-AMINOPYRROLIDINE DIHYDROCHLORIDE

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- then the compound （S -aspartic anhydride was prepared via condensation reaction with L-aspartic acid, ）-l-benzylpyrrolidin-3-amine was obtained from N-formyl-L-aspartic anhydride via acylation, esterification, reduction and ring closing, finally （S） （＋）-3 Aminopyrrolidine dihydro- chloride was obtained through debenzylation with the total yield of 62.8G. The effect of synthesis conditions on （S）-l-benzylpyrrolidin-3-amine was studied. The optimal reaction conditions were found as follows== the yield could reach 71.60/00 when n（KBH4） ： n（H2SO4） ： n（Compound 4）=3 ： 1.5 ： 1 and reacted 6 h at 50 60 ℃. The target compound was confirmed by MS and 1H NMR.