Synthesis and Molecular Design of Water-Soluble, All-Sodium Salts of Heteropolyanion-Supported Organometallic Complexes

杂多阴离子负载有机金属配合物的水溶性全钠盐的合成和分子设计

基本信息

  • 批准号:
    06640735
  • 负责人:
  • 金额:
    $ 1.34万
  • 依托单位:
  • 依托单位国家:
    日本
  • 项目类别:
    Grant-in-Aid for General Scientific Research (C)
  • 财政年份:
    1994
  • 资助国家:
    日本
  • 起止时间:
    1994 至 1995
  • 项目状态:
    已结题

项目摘要

According to the Application for the Grant in 1995, (1) preparation of all-soidum salts of modified Dawson- and Keggin-type heteropolyanion-supports and (2) preparation of organometallic cation-species Cp^<**>Rh^<2+> (Cp^<**>=C_5Me_5) and (3) preparations of the water-soluble, all-sodium salts of heteropolyanion-supported organometallic complexes have been performed. Something new results obtained from this research are as follows :1. Using the sodium salt of Dawson-type modified heteropolyanion Na_9 [P_2W_<15>Nb_3O_<62>] ・23H_2O as a support, the synthetic conditions of the target compound Na_7 [Cp^<**>Rh・P_2W_<15>Nb_3O_<62>] were examined. This compound was formed by refulxing for 4 hr in mixed DMSO/CH_3CN (10 mL/50 mL) under nitrogen. Byproduct NaBF_4 was removed by repeated reprecipitations with DMSO/EtOAc. The purified compound with a formula of Na_7 [Cp^<**>Rh・P_2W_<15>Nb_3O_<62>] ・7DMSO・5H_2O was characterized by full elemental analyzes, TG/DTA,FT-IR,GLC analysis and NMR (^<183>W,^<31>P,^1H,^<13>C) spectroscopy.2. This synthesis was quite different from those of the traditional compound based on the Bu_4N salts.3. By similar method, the preparation of the corresopnding Cp^<**>Rh^<2+> complex supported on Keggin-type Na_7 [SiW_9Nb_3O_<40>] ・16H_2O support was carried out. The target compound was formed by the 4 hr-reaction at 84゚C under nitrogen in mixed DMSO/CH_3CN (7.2 mL/34 mL) solvent. The crude compound obtained here still contained some positional isomers of the supported Cp^<**>Rh^<2+> group. The single isomer was obtained by heating again for 3 hr 84゚C in dry DMSO under nitrogen, followed by purification based on repeated reprecipitations with DMSO/EtOAc. The composition of the target compound was determined as Na_5 [Cp^<**>Rh・SiW_9Nb_3O_<40>] ・3DMSO・2H_2O by characterization with full elemental analysis, TG/DTA,FT-IR and NMR (^<183>W,^<31>P,^1H,^<13>C) spectroscopy.
根据1995年的拨款申请,(1)制备了改性的Dawson和Keggin杂多阴离子载体的全固体盐;(2)制备了有机金属阳离子物种Cp^&lt;**&gt;2+&gt;(Cp^&lt;**&gt;=C_5Me_5);(3)制备了水溶性全钠杂多阴离子负载的有机金属络合物。1.以Dawson型修饰杂多阴离子Na_9[P_2W_&lt;15&gt;Nb_3O_&lt;62&gt;]·23H_2O的钠盐为载体,考察了目标化合物Na_7[Cp^&lt;**&gt;Rh・P_2W_&lt;15&gt;Nb_3O_&lt;62&gt;]的合成条件。该化合物是在DMSO/CH3CN混合液(10毫升/50毫升)中于氮气中回流4小时形成的。副产物NaBF_4用DMSO/EtOAc反复再沉淀除去。通过全元素分析、TG/DTA、FT-IR、GLC分析和核磁共振波谱(^&lt;183&gt;W,^&lt;31&gt;P,^1H,^&lt;13&gt;C)对其结构进行了表征,得到了[Cp^&lt;**&gt;Rh・P_2W_&lt;15&gt;Nb_3O_&lt;62&gt;]·7DMSO·5H2O。这种合成方法与传统的以Bu_4N盐基化合物为基础的合成方法有很大不同。用类似的方法制备了Keggin-型Na_7[SiW_9Nb_3O_(40)&gt;]·16H_2O载体上相应的Cp^&lt;**&gt;Rh^&lt;2+&gt;目标化合物在84゚C氮气存在下,以二甲基亚砜/CH3CN(7.2m L/34 m L)混合溶剂为溶剂,反应4小时。这里得到的粗品仍含有一些支载的Cp^&lt;**&gt;Rh^&lt;2+&gt;基团的位置异构体。单异构体在干燥的二甲基亚砜中氮气中加热3小时84゚C,然后用二甲基亚砜/乙酸乙酯反复再沉淀纯化得到单一异构体。通过全元素分析、TG/DTA、FT-IR和核磁共振(^&lt;183&gt;W,^&lt;31&gt;P,^1H,^&lt;13&gt;C)光谱表征,确定目标化合物的组成为Na5[Cp^&lt;**&gt;Rh·SiW_9Nb_3O_&lt;40&gt;]·3DMSO·2H_2O。

项目成果

期刊论文数量(6)
专著数量(0)
科研奖励数量(0)
会议论文数量(0)
专利数量(0)
K. Nomiya et al.: "The all-sodium salt of a golyoxoanion-sirpported organometallic complex" J. Organometal. Chem.505. 23-28 (1995)
K. Nomiya 等人:“Golyoxoanion-sirpported 有机金属络合物的全钠盐”J. Organometal。
  • DOI:
  • 发表时间:
  • 期刊:
  • 影响因子:
    0
  • 作者:
  • 通讯作者:
K.Nomiya et.al.: "The all-sodium salt of a polyoxoanion-supported organometallic complex Na_7 [Cp^<**>Rh・P_2W_<15>Mb_3O_<62>] ・7DMSO・5H_2O" J.Organometal.Chem.Vol.505. 23-28 (1995)
K.Nomiya 等人:“多氧阴离子负载的有机金属配合物 Na_7 的全钠盐 [Cp^<**>Rh・P_2W_<15>Mb_3O_<62>] ・7DMSO・5H_2O” J.Organometal.Chem .第505卷23-28(1995)
  • DOI:
  • 发表时间:
  • 期刊:
  • 影响因子:
    0
  • 作者:
  • 通讯作者:
K.Nomiya,et al.: "The all-sodium salt of a polyoxoanion-supported organometallic complex,Na_7[Cp^*Rh・P_2W_<15>Nb_3O_<62>]・7DMSO・5H_2O" J.Organometal.Chem.505. 23-28 (1995)
K.Nomiya等人:“多氧阴离子负载的有机金属络合物的全钠盐,Na_7[Cp^*Rh・P_2W_<15>Nb_3O_<62>]・7DMSO・5H_2O” J.Organometal.Chem.505 .23-28 (1995)
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NOMIYA Kenji其他文献

NOMIYA Kenji的其他文献

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{{ truncateString('NOMIYA Kenji', 18)}}的其他基金

Design and Synthesis of Suprarmolecular Metal Complexes Under the Chemical Reaction Fields of Polyoxometalates
多金属氧酸盐化学反应场下超分子金属配合物的设计与合成
  • 批准号:
    22550065
  • 财政年份:
    2010
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for Scientific Research (C)
Synthesis of Novel Functionalized Polyoxometalates Utilizing Chemical Reaction Fields of the Lacunary Species
利用缺位物质的化学反应场合成新型功能化多金属氧酸盐
  • 批准号:
    18550062
  • 财政年份:
    2006
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for Scientific Research (C)
Synthesis of Silver(I) and Gold(I) Complexes Showing a Variety of Spectra of Antimicrobial Activities and Thier Structure-Activity Correlations
显示多种抗菌活性谱及其结构-活性相关性的银 (I) 和金 (I) 配合物的合成
  • 批准号:
    13640566
  • 财政年份:
    2001
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for Scientific Research (C)
Synthesis and Molecular Design of Novel Modified-Heteropolyanions Containing Multicenter Active Sites
含多中心活性位点的新型改性杂多阴离子的合成与分子设计
  • 批准号:
    10640552
  • 财政年份:
    1998
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for Scientific Research (C)
Synthesis and Molecular Design of Heteropolyanion-Supported Organometallics Using Modified Heteropolyanion-Support
使用改性杂多阴离子载体合成和分子设计杂多阴离子负载的有机金属化合物
  • 批准号:
    03640529
  • 财政年份:
    1991
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for General Scientific Research (C)

相似海外基金

Synthesis and Molecular Design of Heteropolyanion-Supported Organometallics Using Modified Heteropolyanion-Support
使用改性杂多阴离子载体合成和分子设计杂多阴离子负载的有机金属化合物
  • 批准号:
    03640529
  • 财政年份:
    1991
  • 资助金额:
    $ 1.34万
  • 项目类别:
    Grant-in-Aid for General Scientific Research (C)
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