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水溶性配体dmPTA和dmoPTA以及配合物[RuClCp(HdmoPTA)(PPh(3))](OSO(2)CF(3))的合成(dmPTA = N,N'-二甲基-1,3,5-三氮杂-7-磷杂金刚烷,dmoPTA = 3,7-二甲基-1,3,7-三氮杂-5-磷杂双环[3.3.1]壬烷,HdmoPTA = 3,7-H-3,7-二甲基-1,3,7-三氮杂-5-磷杂双环[3.3.1]壬烷)。

Synthesis of the water soluble ligands dmPTA and dmoPTA and the complex [RuClCp(HdmoPTA)(PPh(3))](OSO(2)CF(3)) (dmPTA = N,N'-Dimethyl-1,3,5-triaza-7-phosphaadamantane, dmoPTA = 3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane, HdmoPTA = 3,7-H-3,7-Dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane).

作者信息

Mena-Cruz Adrian, Lorenzo-Luis Pablo, Romerosa Antonio, Saoud Mustapha, Serrano-Ruiz Manuel

机构信息

Departamento de Química InorgAnica, Facultad de Química, Universidad de La Laguna, La Laguna, Tenerife, Spain.

出版信息

Inorg Chem. 2007 Jul 23;46(15):6120-8. doi: 10.1021/ic070168m. Epub 2007 Jun 20.

Abstract

The new water-soluble ligand dmPTA(OSO(2)CF(3))(2) (1) (dmPTA = N,N'-dimethyl-1,3,5-triaza-7-phosphaadamantane) has been synthesized by reaction of PTA with MeOSO(2)CF(3) in acetone (PTA = 1,3,5-triaza-7-phosphatricycle[3.3.1.1(3,7)]decane). The reaction of 1 with KOH gave rise to the new water-soluble ligand dmoPTA (3) (dmoPTA = 3,7-dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane) by elimination of the -CH(2)- group located between both NCH(3) units. Compound dmPTA(BF(4))(2) (2) and complex RuClCp(HdmoPTA)(PPh(3)) (4) have also been synthesized, while compounds HdmoPTA(BF(4)) (3a) and RuClCp(dmPTA)(PPh(3)) (5) were characterized but not isolated. The new ligands and the complex have been fully characterized by NMR, IR, elemental analysis, and X-ray crystal structure determination (ligand 1 and complex 4). The synthetic processes for 3 and 4 were studied.

摘要

新型水溶性配体dmPTA(OSO(2)CF(3))(2) (1)(dmPTA = N,N'-二甲基-1,3,5-三氮杂-7-磷杂金刚烷)通过PTA与MeOSO(2)CF(3)在丙酮中反应合成(PTA = 1,3,5-三氮杂-7-磷杂三环[3.3.1.1(3,7)]癸烷)。1与KOH反应通过消除位于两个NCH(3)单元之间的-CH(2)-基团生成新型水溶性配体dmoPTA (3)(dmoPTA = 3,7-二甲基-1,3,7-三氮杂-5-磷杂双环[3.3.1]壬烷)。还合成了化合物dmPTA(BF(4))(2) (2)和配合物RuClCp(HdmoPTA)(PPh(3)) (4),而化合物HdmoPTA(BF(4)) (3a)和RuClCp(dmPTA)(PPh(3)) (5)已被表征但未分离出来。新配体和配合物已通过NMR、IR、元素分析和X射线晶体结构测定(配体1和配合物4)进行了全面表征。研究了3和4的合成过程。

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