Tin(IV) porphyrin functionalization of electrochemically active fluoride-doped tin-oxide (FTO) via Huisgen [3+2] click chemistry

2011 ◽  
Vol 15 (01) ◽  
pp. 75-82 ◽  
Author(s):  
Shiva Prasad ◽  
Mohan Bhadbhade ◽  
Pall Thordarson
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Click Chemistry ◽  
Tin Oxide ◽  
Photoelectron Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Electrochemically Active ◽  
Resolution Mass

A novel tetra-alkyne terminated tin(IV) porphyrin 3 was synthesized in good yields and characterized using NMR spectroscopy, high resolution mass spectrometry and X-ray crystallography, the latter revealing interactions with hexane molecules that stabilize the crystal structure of the tin(IV) porphyrin 3. It was then linked to a conductive fluorine-doped tin oxide (FTO) surfaces using Huisgen [3+2] click chemistry. The attachment of the tin(IV) porphyrin to the FTO surface 6 was characterized by X-ray photoelectron spectroscopy (XPS), indicating the presence of the 1,2,3-triazole unit. Electrochemical measurements of the tin(IV) porphyrin modified FTO surface 7 show that it is still electrochemically active with oxidation (Epa) and reduction peaks (Epc) for the ferricyanide redox couple observed at Epc and Epa of -0.144 and +0.568 V vs. Ag | AgCl respectively, representing a modest shift of ca . +/- 0.1–0.15 V, compared to unmodified FTO.

scholarly journals Synthesis and Crystal Structure of Unexpected (1S,4R,5R,6S)-4-Cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonan-6-yl Acetate

2017 ◽  
Vol 70 (12) ◽  
pp. 1269
Author(s):  
Steven Gareth Williams ◽  
Mohan Bhadbhade ◽  
Roger Bishop ◽  
Alison Thavary Ung
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
X Ray Crystallography ◽  
Ir And Nmr Spectroscopy ◽  
Resolution Mass

The reaction of (–)-β-pinene with KCN under a mild bridged Ritter reaction gave (1S,5R,6S)-2,2,6-trimethyl-3-aza-bicyclo[3.3.1]non-3-en-6-yl acetate that subsequently reacted to provide an unexpected (1S,4R,5R,6S)-4-cyano-2,2,6-trimethyl-3-azabicyclo[3.3.1]nonane-6-yl acetate. The structure of the compound was determined by high-resolution mass spectrometry, and IR and NMR spectroscopy and confirmed by single crystal X-ray crystallography. The compound crystallises in the monoclinic P21 space group, with unit cell parameters a 8.6120 (17), b 7.4570 (15), c 11.189 (2) Å, and β 110.16 (3)°.

Protein interactions of dirhodium tetraacetate: a structural study

2020 ◽  
Vol 49 (8) ◽  
pp. 2412-2416 ◽  
Author(s):  
Giarita Ferraro ◽  
Alessandro Pratesi ◽  
Luigi Messori ◽  
Antonello Merlino
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Protein Interactions ◽  
High Resolution Mass Spectrometry ◽  
Rnase A ◽  
Pancreatic Ribonuclease ◽  
X Ray ◽  
X Ray Crystallography ◽  
Model Protein ◽  
Resolution Mass

The interactions between the cytotoxic paddlewheel dirhodium complex [Rh2(μ-O2CCH3)4] and the model protein bovine pancreatic ribonuclease (RNase A) were investigated by high-resolution mass spectrometry and X-ray crystallography.

scholarly journals Synthesis of spiro[benzo[4,5]imidazo[2,1-b][1,3]thiazole-2,3-thiolane]s via sulfa-Michael/aldol cascade reactions

2019 ◽  
Vol 43 (1-2) ◽  
pp. 63-66 ◽  
Author(s):  
Jiaying Lei ◽  
Xinliang Fu ◽  
Yulin Huang ◽  
Xiaofang Li
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Cascade Reactions ◽  
Cascade Reaction ◽  
Crystallographic Analysis ◽  
X Ray ◽  
Resolution Mass

The sulfa-Michael/aldol cascade reaction of ( Z)-2-arylmethylidene-benzo[4,5]imidazo[2,1- b]thiazol-3(2H)-ones and 1,4-dithiane-2,5-diol afforded novel 2-aryl-4-hydroxy-spiro[benzo[4,5]imidazo[2,1- b][1,3]thiazole-2,3-thiolan]-3-ones in moderate yields. The structures of all the products were characterized thoroughly by nuclear magnetic resonance, infrared and high-resolution mass spectrometry together with X-ray crystallographic analysis.

Improved Access to 1,8-Dichloro-10-(ethynyl)anthracene: A Useful Building Block for (Semi-)rigid Organic Frameworks

Synthesis ◽  
2018 ◽  
Vol 50 (10) ◽  
pp. 2009-2018
Author(s):  
Jan-Hendrik Lamm ◽  
Philipp Niermeier ◽  
Leif Körte ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Building Block ◽  
High Resolution Mass Spectrometry ◽  
Cross Coupling ◽  
Easy Access ◽  
Coupling Reactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cross Coupling Reactions ◽  
Resolution Mass

An easy access to 1,8-dichloro-10-(ethynyl)anthracene is reported, which is widely applicable for building up rigid linkers between two 1,8-dichloroanthracene units. For this, 1,8-dichloroanthren-10(9H)-one was reacted with ethynylmagnesium bromide in the presence of CeCl3; the yield was 65%. This building block was used as a substrate in (cross-)coupling reactions and some examples of linked 1,8-dichloroanthracen-10-yls (e.g., 1,8-bis[(1,8-dichloroanthracen-10-yl)-ethynyl]naphthalene or 1,2-bis[(1,8-dichloroanthracen-10-yl)ethynyl]-benzene) were synthesized in good to moderate yields. Linked 1,8-dichloroanthracen-10-yl derivatives were also synthesized by cross-coupling reactions using 10-bromo-1,8-dichloroanthracene and doubly ethynyl-substituted substrates. Linkers between the 1,8-dichloroanthracene units were: butadiynediyl, dimethylsilyldiethynyl, octa-1,7-diyne-1,8-diyl, propane-1,3-diylbis(dimethylsilyl)diethynyl, benzene-1,2-diethynyl, naphthalene-1,8-diyldiethynyl, and anthracene-1,8-diyldiethynyl. The new anthracene compounds were characterized by NMR spectroscopy, high-resolution mass spectrometry, and, in part, by X-ray diffraction experiments.

scholarly journals One-pot synthesis and the structure study of a new indoline spiropyran with cationic substituent

2019 ◽  
Vol 488 (5) ◽  
pp. 498-503
Author(s):  
A. D. Pugachev ◽  
A. S. Kozlenko ◽  
M. B. Lukyanova ◽  
B. S. Lukyanov ◽  
V. V. Tkachev ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Single Crystals ◽  
High Resolution Mass Spectrometry ◽  
Structure Study ◽  
One Pot ◽  
X Ray ◽  
One Pot Synthesis ◽  
High Resolution Mass ◽  
Resolution Mass

One-pot synthesis and the structure study of a new salt spiropyran of indoline series containing 2H-chromenic vinyl-3H-indolium fragment as a substituent at the position 8 are described. The structure was confirmed by the method of NMR 1H and 13C spectroscopy, IR and high-resolution mass spectrometry. The single crystals of the compound were investigated by X-ray analysis. The structure was compared with the previously known isostructural analogue [10].

scholarly journals Synthesis, Crystal Structure and Interaction with Bovine Serum Albumin (BSA) of Two α-Aminophosphonic Acids Derivatives

2019 ◽  
pp. 1-7
Author(s):  
Wei Huang ◽  
Wen-Ling Wang
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Binding Constants ◽  
Ionization Mass ◽  
Monoclinic System ◽  
X Ray ◽  
X Ray Crystallography ◽  
Aminophosphonic Acids ◽  
Amino Phosphonate ◽  
Ft Ir

Two α-amino-phosphonate derivatives (1 & 2) were synthesized and their compositions and structures were characterized by Elemental Analysis (EA), FT-IR Spectrascopy (FT-IR), Electrospray Ionization Mass Spectrometry (ESI-MS), Nuclear Magnetic Resonance (NMR, 1H, 13C and 31P) and X-ray crystallography. Compound 1 & 2 were crystallized in monoclinic system with the space group P2(1)/n and P2(1)/c, respectively. The interaction effects of two α-aminophosphonate derivatives (1 & 2) with BSA were investigated and the binding constants were 1.07 × 104 M-1, 1.68 × 104 M-1, respectively. Besides, the values of n were indicated that 1:1 complex was formed between BSA and 1&2.

Structural Identification of Products from the Chloromethylation of Salicylaldehyde

Synlett ◽  
2018 ◽  
Vol 30 (01) ◽  
pp. 44-48 ◽  
Author(s):  
Muhammad Bala ◽  
Ebrahim Kadwa ◽  
Holger Friedrich
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
High Resolution Mass Spectrometry ◽  
Structural Identification ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Ir Spectroscopic ◽  
Resolution Mass

In the functionalization of salicylaldehyde to give 5-(chloromethyl)salicylaldehyde, two byproducts [5-(hydroxymethyl)salicylaldehyde and 5,5′-methylenebis(salicylaldehyde)] were also isolated. ­Detailed characterizations and structural analyses of all three products by single-crystal X-ray diffraction, multinuclear NMR spectroscopy, high-resolution mass spectrometry, and IR spectroscopic techniques are presented and discussed. A strategy is presented for the preferential isolation of the two byproducts through column chromatography.

Synthesis, crystal structure, aggregation-induced emission (AIE) and electroluminescence properties of a novel emitting material based on pyrrolo[3,2-b]pyrrole

2020 ◽  
Vol 8 (40) ◽  
pp. 14208-14218
Author(s):  
Hongbo Wang ◽  
Jinnan Huo ◽  
Hongbo Tong ◽  
Xuehong Wei ◽  
Ying Zhang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Donor Group ◽  
Aggregation Induced Emission ◽  
X Ray ◽  
X Ray Crystallography

A novel electroluminescent material based on pyrrolo[3,2-b]pyrrole as skeleton and donor group and dimesitylborons as accept groups has been synthesized and characterized by elemental analysis, mass spectrometry, NMR spectroscopy and X-ray crystallography.

Synthesis of 1,2,3-triazole-substituted 6,7-dihydroindolizin-8(5H)-one derivatives mediated by Selectfluor

2019 ◽  
Vol 43 (5-6) ◽  
pp. 179-183
Author(s):  
Yulin Huang ◽  
Jiaying Lei ◽  
Xinliang Fu ◽  
Wenlin Xie ◽  
Xiaofang Li
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Crystallographic Analysis ◽  
X Ray ◽  
High Resolution Mass ◽  
Moderate Yield ◽  
Resolution Mass

The 1,2,3-triazole and 1 H-1,2,3-benzotriazole-substituted 6,7-dihydroindolizin-8(5 H)-one derivatives were synthesized by the reaction of ( E)-7-(arylmethylidene)-6,7-dihydroindolizin-8(5 H)-ones with 1,2,3-triazole and 1 H-1,2,3-benzotriazole in the presence of Selectfluor in moderate yield. The structures of all the products were characterized thoroughly by nuclear magnetic resonance, infrared, and high-resolution mass spectrometry together with X-ray crystallographic analysis.

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