One-Pot Mechanochemical Synthesis of Metal Complexes from Precursor Without Isolating the Ligand

2021 ◽  
Author(s):  
GETINET TAMIRU TIGINEH
2014 ◽  
Vol 18 (01n02) ◽  
pp. 115-122 ◽  
Author(s):  
Srinivas Banala ◽  
Klaus Wurst ◽  
Bernhard Kräutler

We report here the preparation (in "one-pot") of a tetra-β″-sulfoleno-meso-aryl-porphyrin in about 80% yield by using an optimized modification of Lindsey's variant of the Adler–Longo approach. The Zn ( II )-, Cu ( II )- and Ni ( II )-complexes of the symmetrical porphyrin were prepared and characterized spectroscopically. Crystal structures of the fluorescent Zn ( II )- and of the non-fluorescent Ni ( II )-tetra-β″-sulfoleno-meso-aryl-porphyrinates showed the highly substituted porphyrin ligands to be nearly perfectly planar. The Zn ( II )-complex of this porphyrin has been used as a thermal precursor of a reactive diene, and — formally — of lateral and diagonal bis-dienes, of a tris-diene and of a tetra-diene, which all underwent [4 + 2]-cycloaddition reactions in situ with a range of dienophiles. Thus, the tetra-β″-sulfoleno-meso-aryl-porphyrin and its metal complexes represent reactive building blocks, "programmed" for the syntheses of symmetrical and highly functionalized porphyrins.


2020 ◽  
Vol 8 (8) ◽  
pp. 3114-3125
Author(s):  
Lori Gonnet ◽  
Christiane André-Barrès ◽  
Brigitte Guidetti ◽  
Alain Chamayou ◽  
Christophe Menendez ◽  
...  

1991 ◽  
Vol 10 (3) ◽  
pp. 820-823 ◽  
Author(s):  
Claudio. Bianchini ◽  
Andrea. Meli ◽  
Maurizio. Peruzzini ◽  
Francesco. Vizza ◽  
Fiorella. Bachechi

2014 ◽  
Vol 16 (3) ◽  
pp. 1374-1382 ◽  
Author(s):  
Michael Ferguson ◽  
Nicola Giri ◽  
Xu Huang ◽  
David Apperley ◽  
Stuart L. James

2004 ◽  
Vol 7 (2) ◽  
pp. 249-252 ◽  
Author(s):  
Zhikun Wu ◽  
Guoqiang Yang ◽  
Qingqi Chen ◽  
Jingang Liu ◽  
Shiyong Yang ◽  
...  

Author(s):  
D.T. Biradar ◽  

Objective: Many methods can be found in literature for the synthesis a Oxazines and Thiazines. Few are reported for one-pot multi component cyclo-condensation of an alkayane urea / Thiourea and Aldehyde to 2- amino-4H-1, 3-Oxazines or Thiazines. Different catalysts are reported like Trifluoro-acetic acid, glacial acetic acid under reflux condition Mandal and Co-workers have utilized perchloric acid (HClO4) supported on silica gel as catalyst under solvent free condition ytterbium trifluorate [Yb(OTF)3] plays role of Lewis acid. It is also used in several Diel’s-Alder cyclo-addition reactions. Inspired these observations, development of simple effective synthetic strategy for the synthesis of 2-amino-4H-1, 3-Oxazium & Thiazines was attempted. Material and Methods: One pot multi-component synthesis of Schiff’s base as new ligand an their complexes with Ni, Fe, Co and Cu and developed using 2-amino-4H-1,3 Oxazines /Thiazines and substituted Aldehydes, different catalyst are used to synthesize of 2-amino 4H-1,3 Oxazines. Its characterization is confirmed by taking IR, NMR spectra. The Schiff’s base act as ligand is bidentate, when it is treated to metal complexes in 1:1 ratio (metal: ligand) complexes are formed. Result: By using the bioactive molecules like 2-amino-4H-1, 3 Oxazine / Thiazines, Schiff’s Bases can be synthesized by using different aldehydes. These Schiff’s Bases has antitumor, antipyretic, anti-inflammatory property. And these Schiff’s bases treated with bioactive metals like Co, Fe, Cu, Zn which enhances their bio-activity. Conclusion: All these synthesized Schiff’ Bases and their metal complexes having bioactive properties.


2020 ◽  
Author(s):  
Naoki Kamo ◽  
Tomoya Kujirai ◽  
Hitoshi Kurumizaka ◽  
Hitoshi Murakami ◽  
Gosuke Hayashi ◽  
...  

For epigenetics research, preparing homogeneous proteins bearing site-specific posttranslational modifications (PTMs) is essential to understand the behavior of chromatin. Total chemical protein synthesis is a very powerful method to obtain target proteins with various modifications at site-specific positions. To produce large proteins efficiently, one-pot ligation of multiple peptide fragments was previously reported through repetitive deprotection of protecting groups for N-terminal Cys with palladium complexes. However, this method demanded more than a catalytic amount of metal complexes, and, in general, it had been challenging to achieve catalytic cycles of metal complexes especially for reactions on proteins. Here, we report an efficient and facile method of chemical protein synthesis using Ru catalyst. The use of 10–20 mol% of Ru complexes enabled us to remove the protecting groups on peptides or proteins under peptide ligation conditions, and this complex showed more than 50-fold activity compared to the previous palladium complexes due to the great stability toward thiol moieties. By using this Ru catalyst, we accomplished total chemical synthesis of linker histone H1.2 (212 amino acids) and heterochromatin protein 1a (HP1a) (191 amino acids), which are important components of heterochromatin, through one-pot multiple peptide ligation. This method prompted the preparation of H1.2 and HP1a bearing various patterns of PTMs. Moreover, we found that R53Cit at H1.2 reduced its binding affinity toward nucleosomes and four consecutive phosphorylations at N-terminus HP1a controlled its binding ability against DNA. We envisage that homogeneously modified proteins prepared by our method would facilitate epigenetics research and be applied for the elucidation of various biological phenomena.


2013 ◽  
Vol 85 (2) ◽  
pp. 315-327 ◽  
Author(s):  
Christina D. Polyzou ◽  
Constantinos G. Efthymiou ◽  
Albert Escuer ◽  
Luís Cunha-Silva ◽  
Constantina Papatriantafyllopoulou ◽  
...  

The importance of 3d/4f-metal cluster chemistry is outlined, and the employment of 2-pyridyl ketone- and 2-pyridyl oxime-based ligands for the preparation of low-nuclearity NiII/LnIII complexes (Ln = lanthanide) is reviewed. The synthetic utility of the “metal complexes as ligands” and “one-pot” approaches is critically discussed. The small nuclearity of the products permits the in-depth analysis of their magnetic properties.


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