Synthesis and characterization of dendritic platinum bisferrocenylacetylide complexes

2012 ◽  
Vol 90 (3) ◽  
pp. 278-289
Author(s):  
Qing Han ◽  
Li-Jun Chen ◽  
Hai-Bo Yang ◽  
Quan-Jie Li ◽  
Jiuming He ◽  
...  

A series of new dendritic platinum bisferrocenylacetylide complexes have been synthesized utilizing the coupling reaction of trans-Pt complexes with C–H bonds in alkynes as key steps. These new bimetallic dendrimers were fully characterized by multinuclear NMR (1H, 13C, and 31P) and mass spectrometry (MALDI-TOF-MS and CSI-TOF-MS). Electrochemical studies of these complexes were carried out and revealed that all of the redox moieties are stable, independent, and electrochemically active. In addition, all metallodendrimers show one-electron reaction responses, and the increased sizes of these complexes did not exhibit a dramatic influence on the diffusion coefficient.

2017 ◽  
Vol 75 (6) ◽  
pp. 2657-2670
Author(s):  
Albert Morell Garcia ◽  
Francisco Medina Cabello ◽  
Antonio Torrelles Nogués

1999 ◽  
Vol 561 ◽  
Author(s):  
R.C. Advincula ◽  
S. Inaoka ◽  
M. Park ◽  
D. Phillips ◽  
D.M. Shin

ABSTRACTIn this report, we describe our initial synthesis and characterization of mono-functional and bi-functional dibromoalkyl oligothiophenes to achieve amphiphilicity and telechelic functionality. Oligothiophenes are an important class of organic materials for opto-electronic devices and display applications. We have mono-functionalized oligothiophenes by the synthesis of a quinquethiophene bromoalkyl derivative. A bi-functional sexithiophene was derived primarily by the symmetrical coupling of terthiophene derivatives. Both were synthesized using Grignard coupling and lithiation reaction methodologies. UV-Vis, IR, NMR, MALDI-TOF-MS, and DSC confirmed the structure and physical properties of the oligomers. In addition, we have also synthesized an amphiphilic diamine derivative from the reaction of hexamethylenediamine with a bromoalkyl terthiophene derivative. Using photoluminescence, the photophysical properties of the oligomers were found to be that of typical oligothiophenes. Processing as ultrathin films for devices is currently being investigated.


2007 ◽  
Vol 61 (6) ◽  
pp. 333-341
Author(s):  
Jasna Vukovic ◽  
Slobodan Jovanovic ◽  
Manfred Lechner

In this work, MALDI-TOF mass spectrometry was used for the characterization of aliphatic hyperbranched polyesters (AHBP), synthesized from 2,2-bis(hydroxymethyl)propionic acid (bis-MPA) and di-trimethylolpropane. From the obtained results it was concluded that it was not possible to take complete advantages of MALDI-TOF MS in this particular case, since the AHBP used in this work were polydisperse. The intensity of the signals from the high mass tail of these samples (pseudo generation higher than four) was underestimated and insufficient to distinguish it from the baseline and to use it for the analysis of the spectra. As a consequence of that, lower values of the Mn were obtained. At the same time, Mw were also underestimated, which led to very low values of the polydispersity index. On the other hand, it was possible to obtain molar masses of individual molecules from the MALDI-TOF mass spectra of AHBP and to qualitatively determine the extent of cyclization (side reactions) at each degree of polymerization. Using the adequate set of equations and results obtained from MALDI-TOF mass spectra of AHBP, every signal from the spectra was identified. The obtained results show that formation of poly(bis-MPA), intramolecular esterification and intramolecular etherification occurred as side reactions during the synthesis of these polyesters. The relative amount of the cycles increases with the number of pseudo generation (from the second up to the fifth pseudo generation). It was also observed that the relative proportion of the signals which represent cyclic structures increases with the increasing degree of polymerization. In this work the basic principles of MALDI-TOF MS are also presented, as well as, a review of adequate published articles.


Author(s):  
N. SRINIVASAN ◽  
CAROL A. HANEY ◽  
JONATHAN S. LINDSEY ◽  
WENZHU ZHANG ◽  
BRIAN T. CHAIT

We investigated the utility of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) for analyzing porphyrinic compounds using a variety of different synthetic porphyrins, azaporphyrins, phthalocyanines and multiporphyrin arrays. Comparisons of spectra obtained from these analytes deposited either as neat samples or codeposited with neutral or acidic matrices have been made with the goal of identifying conditions that yield minimal demetalation, transmetalation, adduct formation and fragmentation. It was found that the molecular masses of many porphyrins can be successfully measured from neat sample preparations and do not require a matrix to facilitate desorption and ionization, although the measurement of large multiporphyrin arrays was facilitated by the use of matrices. Demetalation of magnesium porphyrins occurred in the presence of acidic matrices, but not with neutral matrices such as 1,4-benzoquinone. Positive ion spectra were obtained for each compound and negative ion spectra were also collected for the azaporphyrins and phthalocyanines. Examination of selected samples (prepared neat, with 1,4-benzoquinone, 2,3,5,6-tetrachloro-1,4-benzoquinone or α-cyano-4-hydroxycinnamic acid) showed that the dominant process of ionization involved oxidation yielding the radical cation M+· rather than the protonated molecule [M+H]+. MALDI-TOF-MS is shown to be a powerful analytical tool for the characterization of diverse synthetic porphyrinic compounds.


2012 ◽  
Vol 554-556 ◽  
pp. 640-643
Author(s):  
Wei Zhang ◽  
Wu Biao Duan ◽  
Zhen Xin Wang

A novel tetra-substituted zinc phthalocyanine 4 [ZnPcNHCOCH2(PEG)5NH2] was synthesized from 4-nitrophthalonitrile by using a four-step procedure. The compound has been characterized by UV–Visible, fluorescence, IR, 1H NMR spectra and MALDI-TOF MS, and the satisfactory result has been obtained. Most importantly, this compound is soluble in many solvents including CHCl3, CH2Cl2, DMF, DMSO, THF and water.


1996 ◽  
Vol 110 (1) ◽  
pp. 231-240 ◽  
Author(s):  
Bernd Trathnigg ◽  
Bernhard Maier ◽  
Günther Schulz ◽  
Ralph-Peter Krüger ◽  
Ulrich Just
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