手性仲丁胺的制备拆分和光学纯度的测定 |
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引用本文: | 车超,代星,毛淑芬,徐彦军,覃兆海.手性仲丁胺的制备拆分和光学纯度的测定[J].有机化学,2003,23(4):390-392. |
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作者姓名: | 车超 代星 毛淑芬 徐彦军 覃兆海 |
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作者单位: | 中国农业大学应用化学学院,北京,100094 |
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摘 要: | 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%.
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关 键 词: | 仲丁胺 异构体 酒石酸 晶体结构 离子交换树脂 |
修稿时间: | 2002年7月1日 |
Preparative Resolution and Enantiomeric Purity Assessment of sec- Butylamine |
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Institution: | College of Applied Chemistry,China Agricultural University |
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Abstract: | 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. |
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Keywords: | sec butylamine resolution enantiomeric purity |
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