摘要
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.
出处
《精细石油化工》
CAS
CSCD
北大核心
2013年第3期35-38,共4页
Speciality Petrochemicals
基金
"国家重大新药创制"科技重大专项资助(2009JX090301-007)
上海市优秀学科带头人计划项目(09XD1423100)