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格氏试剂RMgCl在四氢呋喃中的制备。

Constitution of Grignard reagent RMgCl in tetrahydrofuran.

作者信息

Sakamoto S, Imamoto T, Yamaguchi K

机构信息

Chemical Analysis Center and Faculty of Science, Chiba University, Yayoi-cho, Inage-ku, Chiba 263-8522, Japan.

出版信息

Org Lett. 2001 Jun 14;3(12):1793-5. doi: 10.1021/ol010048x.

Abstract

The constitution of Grignard reagent, RMgCl (R = Me, tBu, Ph or benzyl), was investigated in the solid state by means of X-ray crystallography and in THF by coldspray ionization mass spectrometry (CSI-MS). Three types of crystal structures, (a) Mg2(mu-Cl3)(THF)6RMgCl2(THF), (b) R2Mg4Cl6(THF)6, and (c) 2Mg2(mu-Cl3)(THF)6[R4Mg2Cl2]2-, were identified, and MeMg2(mu-Cl3)(THF)4-6 were detected as major species of MeMgCl in solution.

摘要

通过X射线晶体学在固态下以及通过冷喷雾电离质谱(CSI-MS)在四氢呋喃(THF)中对格氏试剂RMgCl(R = 甲基、叔丁基、苯基或苄基)的组成进行了研究。确定了三种晶体结构,(a)Mg2(μ-Cl3)(THF)6·RMgCl2(THF),(b)R2Mg4Cl6(THF)6,以及(c)2Mg2(μ-Cl3)(THF)6·[R4Mg2Cl2]2-,并且在溶液中检测到MeMg2(μ-Cl3)(THF)4-6是MeMgCl的主要物种。

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