化学试剂
化學試劑
화학시제
CHEMICAL REAGENTS
2010年
4期
299-301
,共3页
叶玲娅%曹飞%武红丽%杨颖%周佳栋%韦萍
葉玲婭%曹飛%武紅麗%楊穎%週佳棟%韋萍
협령아%조비%무홍려%양영%주가동%위평
2S,7S-二氨基辛二酸%BPB-Ni(Ⅱ)-Gly复合物%席夫碱%不对称合成
2S,7S-二氨基辛二痠%BPB-Ni(Ⅱ)-Gly複閤物%席伕堿%不對稱閤成
2S,7S-이안기신이산%BPB-Ni(Ⅱ)-Gly복합물%석부감%불대칭합성
2S,7S-diaminosuberic acid%BPB-Ni(Ⅱ)-Gly complex%Schiff base%asymmetric synthesis
以S-2-N-(N′-苄基-S-脯氨酰)-氨基二苯甲酮-镍(Ⅱ)-甘氨酸(BPB-Ni(Ⅱ)-Gly)复合物为手性助剂,与1,4-二溴丁烷反应制备了标题化合物.探讨了反应时间以及反应物配比对反应产率影响,确定了最佳反应条件:BPB-Ni(Ⅱ)-Gly复合物与1,4-二溴丁烷的物质的量比为1∶0.5,反应时间为10 min.2S,7S-二氨基辛二酸的总产率为63%.同时用核磁共振、高分辨质谱及旋光技术对产物进行了表征.
以S-2-N-(N′-芐基-S-脯氨酰)-氨基二苯甲酮-鎳(Ⅱ)-甘氨痠(BPB-Ni(Ⅱ)-Gly)複閤物為手性助劑,與1,4-二溴丁烷反應製備瞭標題化閤物.探討瞭反應時間以及反應物配比對反應產率影響,確定瞭最佳反應條件:BPB-Ni(Ⅱ)-Gly複閤物與1,4-二溴丁烷的物質的量比為1∶0.5,反應時間為10 min.2S,7S-二氨基辛二痠的總產率為63%.同時用覈磁共振、高分辨質譜及鏇光技術對產物進行瞭錶徵.
이S-2-N-(N′-변기-S-포안선)-안기이분갑동-얼(Ⅱ)-감안산(BPB-Ni(Ⅱ)-Gly)복합물위수성조제,여1,4-이추정완반응제비료표제화합물.탐토료반응시간이급반응물배비대반응산솔영향,학정료최가반응조건:BPB-Ni(Ⅱ)-Gly복합물여1,4-이추정완적물질적량비위1∶0.5,반응시간위10 min.2S,7S-이안기신이산적총산솔위63%.동시용핵자공진、고분변질보급선광기술대산물진행료표정.
2S,7S-Diaminosuberic acid was asymmetrically synthesized by reacting Gly-Ni-2[N-(N′-benzylprolyl)amino]benzophenone as the chiral auxiliary with 1,4-dibromobutane.The effect of the molar ratio of Ni(Ⅱ) complexes of glycine Schiff base to 1,4-dibromobutane and the reaction time on the yield of intermediates was investigated.The optimal reaction conditions were determined as follows:a molar ratio of 1∶0.5,and a reaction time of 10 min.The yield of 2S,7S-diaminosuberic acid was 63%.All products were characterized by NMR,MS,and optical rotation technique.