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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (4): 390-392. 上一篇    下一篇

研究论文

手性仲丁胺的制备拆分和光学纯度的测定

车超;代星;毛淑芬;徐彦军;覃兆海   

  1. 中国农业大学应用化学学院
  • 发布日期:2003-04-25

Preparative Resolution and Enantiomeric Purity Assessment of sec- Butylamine

Che Chao;Dai Xing;Mao ShuFen;Xu YanJun;Qin ZhaoHai   

  1. College of Applied Chemistry,China Agricultural University
  • Published:2003-04-25

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被引次数

28 | 2

为了获取仲丁胺的两种光学纯对映异构体，采用D-或L-酒石酸作为拆分试剂， 经过多次结晶，分别得到S-(+)-仲丁胺·乙-(+)-酒石酸盐和R-(-)-仲丁胺·D-(-) -酒石酸盐晶体，从而成功实现了其分离．产物的光学纯度通过用光活性(R)-联萘 酚磷酰氯衍生成(R)-联萘酚磷酰胺后，经^31P NMR测定，o_p_＞99％，拆分剂D-或 L-酒石酸经过强酸型阳离于交换树脂(001×7×7型)方便回收，回收率＞80％．

关键词: 仲丁胺, 异构体, 酒石酸, 晶体结构, 离子交换树脂

Using D- or L-tartaric acid as resolving agent, a method was established to resolve sec-butylamine intoboth of its pure enantiomers with o. p. > 99% , and the enantiomeric purities were assessed by P NMR after the formation of the cyclic phosphoramidate with 7?-BINOPCl. The resolving agents were conveniently recovered by passing the acidified solution through a sulfonie resin (001x7x7) column with > 80% recovery yield.

Key words: buytlamine, ISOMER, TARTARIC ACID, CRYSTAL STRUCTURE, ION EXCHANGE RESINS

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