scholarly journals A Facile Strategy for the High Yielding, Quantitative Conversion of Polyglycol End-Groups to Amines

Polymers ◽  
2021 ◽  
Vol 13 (9) ◽  
pp. 1403
Author(s):  
Jie Yan ◽  
Paula Facal Marina ◽  
Anton Blencowe
Keyword(s):  
Nmr Spectroscopy ◽  
Ethylene Glycol ◽  
Slight Reduction ◽  
Poly Ethylene Glycol ◽  
End Groups ◽  
Poly Ethylene ◽  
Poly Propylene ◽  
Work Up ◽  
End Group ◽  
Tof Ms

Amino end-group functionalised polyglycols are important intermediates in the synthesis of sophisticated polymeric architectures and biomaterials. Herein, we report a facile strategy for the end-group conversion of hydroxyl-terminated polyglycols to amino-terminated polyglycols in high isolated yields and with excellent end-group fidelity. Following traditional conversion of polyglycol hydroxyl end-groups to azides via the corresponding mesylate, reduction with zinc in the presence of ammonium chloride afforded a range of amino end-group functionalised poly(ethylene glycol) and poly(propylene glycol) homopolymers and copolymers with isolated yields of 82–99% and end-group conversions of >99% as determined by NMR spectroscopy and MALDI ToF MS. Furthermore, this process is applicable to a sequential reagent addition approach without intermediate polymer isolation steps with only a slight reduction in yield and end-group conversion (95%). Importantly, a simple work-up procedure provides access to high purity polyglycols without contamination from other reagents.

Synthesis of Poly(ethylene glycol) Derivatives

2013 ◽  
Vol 750-752 ◽  
pp. 1674-1677
Author(s):  
Hai Yun Chen ◽  
Yu Kai Shan ◽  
Yu Yue Qin ◽  
Guo Xian Zhou ◽  
Ming Long Yuan
Keyword(s):  
Nmr Spectroscopy ◽  
Ethylene Glycol ◽  
Biologically Active ◽  
Poly Ethylene Glycol ◽  
H Nmr ◽  
End Groups ◽  
Poly Ethylene ◽  
Ethylene Glycol Derivatives

To expand the extent of conjugation with biologically active molecules (biopolymers, peptides, drugs, etc.) and biomaterial substrates, we synthesized a serial of poly (ethy1ene glycol) (PEG) derivatives (PEG-2000-NH2, MPEG-1200-NH2, and APEG-1200-NH2) in three efficient steps. The end groups were characterized by 1H NMR spectroscopy.

scholarly journals Synthesis and MALDI-ToF characterization of dendronized poly(ethylene glycol)s

2013 ◽  
Vol 49 (spe) ◽  
pp. 45-55 ◽  
Author(s):  
Brittany K. Myers ◽  
Joanna E. Lapucha ◽  
Scott M. Grayson
Keyword(s):  
Ethylene Glycol ◽  
Poly Ethylene Glycol ◽  
Maldi Tof ◽  
Product Characterization ◽  
End Groups ◽  
Linear Poly ◽  
Mass Spectrometric Approach ◽  
Poly Ethylene ◽  
End Group

Well-defined hybrids of linear poly(ethylene glycol)s (PEGs) and dendritic polyesters were prepared via the dendronization of the alcohol end groups of the mono and difunctional linear PEGs. Though useful for rudimentary product characterization, GPC and NMR could not verify the overall structural purity of these linear-dendritic hybrids. On the other hand, the detailed data provided by MALDI-ToF mass spectrometry enabled confirmation of the high structural purity of the dendronized PEGs at each step of the dendronization procedure. The well-defined number of functionalities on these dendronized PEGs, renders them particularly useful for research in the biomedical sphere where functionality and purity are of the utmost importance. The MALDI-ToF mass spectrometric approach described herein represents a valuable technique for detailed monitoring of these dendronization reactions, as well as a variety of other polymer end group modifications.

scholarly journals Immobilization of metalloporphyrin on functionalized SBA-15 nanoporous silica

2016 ◽  
Vol 11 (4) ◽  
Author(s):  
Nurafiqah Saadon ◽  
Salasiah Endud ◽  
Mohd Bakri Bakar ◽  
Mahsa Khoshkhooy Yazdi
Keyword(s):  
Nmr Spectroscopy ◽  
Ethylene Glycol ◽  
Sol Gel ◽  
Soret Band ◽  
Nanoporous Silica ◽  
Poly Ethylene Glycol ◽  
Metal Source ◽  
Heterogenous Catalyst ◽  
Poly Ethylene ◽  
Poly Propylene

SBA-15 nanoporous silica was prepared by cooperation assembly of tetraethylorthosilicate  precursor in the presence of poly (ethylene glycol)–block- poly (propylene glycol)–block- poly (ethylene glycol) copolymer surfactant and functionalized with (3-aminopropyl) triethoxysilane (APTES) via sol-gel reaction to obtain APTES-SBA-15. Tetra-(p-chlorophenyl) porphyrin (TClPP) was synthesized using modified Alder- Longo method. Zinc was inserted into the TClPP using zinc acetate as a metal source The existance of zinc in porphyrin was confirmed by the appearance of Soret band and Q band in UV- vis spectra. ZnTClPP was also characterized using FTIR and NMR spectroscopy SBA-15 was modified with APTES to immobilize the metalloporphyrin on SBA-15 surface. The product (NH-SBA-15 ZnP) can be used as a heterogenous catalyst in various reactions. The formation of this material was confirmed by FTIR spectroscopy, XRD and BET adsorption. 

Chemical Structures of Liquid Poly(ethylene glycol)s with Different End Groups at Buried Polymer Interfaces

2006 ◽  
Vol 39 (26) ◽  
pp. 9396-9401 ◽  
Author(s):  
Mark A. Even ◽  
Chunyan Chen ◽  
Jie Wang ◽  
Zhan Chen
Keyword(s):  
Ethylene Glycol ◽  
Polymer Interfaces ◽  
Poly Ethylene Glycol ◽  
Chemical Structures ◽  
End Groups ◽  
Poly Ethylene

scholarly journals End group functionalization of poly(ethylene glycol) with phenolphthalein: towards star-shaped polymers based on supramolecular interactions

2014 ◽  
Vol 10 ◽  
pp. 2263-2269 ◽  
Author(s):  
Carolin Fleischmann ◽  
Hendrik Wöhlk ◽  
Helmut Ritter
Keyword(s):  
Ethylene Glycol ◽  
Cycloaddition Reaction ◽  
Supramolecular Interactions ◽  
Poly Ethylene Glycol ◽  
Naked Eye ◽  
Vis Spectroscopy ◽  
End Group Functionalization ◽  
Interesting Approach ◽  
Poly Ethylene ◽  
End Group

The synthesis of a new phenolphthalein azide derivative, which can be easily utilized in polymer analogous reactions, is presented. The subsequent cycloaddition reaction with propargyl-functionalized methoxypoly(ethylene glycol) yielded polymers bearing phenolphthalein as the covalently attached end group. In presence of per-β-cyclodextrin-dipentaerythritol, the formation of stable inclusion complexes was observed, representing an interesting approach towards the formation of star shaped polymers. The decolorization of a basic polymer solution caused by the complexation was of great advantage since this behavior enabled following the complex formation by UV–vis spectroscopy and even the naked eye.

A chitosan/poly(ethylene glycol)-ran-poly(propylene glycol) blend as an eco-benign separator and binder for quasi-solid-state supercapacitor applications

2019 ◽  
Vol 3 (3) ◽  
pp. 760-773 ◽  
Author(s):  
M. Raja ◽  
Balaji Sadhasivam ◽  
Janraj Naik R ◽  
Dhamodharan R ◽  
Kothandaraman Ramanujam
Keyword(s):  
Activated Carbon ◽  
Solid State ◽  
Ethylene Glycol ◽  
Propylene Glycol ◽  
Tamarindus Indica ◽  
Poly Ethylene Glycol ◽  
Active Electrode ◽  
Poly Ethylene ◽  
Poly Propylene ◽  
Supercapacitor Applications

In this study chitosan/poly(ethylene glycol)-ran-poly(propylene glycol) blend was developed as separator and binder for supercapacitor (SC) applications. The activated carbon (ACTS-900) derived fromTamarindus indicaseeds is used as active electrode material.

scholarly journals Sizing and Thermal Stability of Prepared Tetraaminophthalocyaninatocopper(II) Derivatives-grafted Polymers

2016 ◽  
Vol 13 (2) ◽  
pp. 221-234
Author(s):  
Baghdad Science Journal
Keyword(s):  
Thermal Stability ◽  
Ethylene Glycol ◽  
Group Analysis ◽  
Condensation Polymerization ◽  
Grafted Polymers ◽  
Poly Ethylene Glycol ◽  
Molecular Weights ◽  
Poly Ethylene ◽  
Thermal Stability Of ◽  
End Group

Different polymers were prepared by condensation polymerization of sebacic anhydride and adipic anhydride with ethylene glycol and poly(ethylene glycol). Their number average molecular weights were determined by end group analysis. Then, they were grafted on the prepared phthalocyaninatocopper(II) compounds with the general formula (NH2)4PcCu(II) having amino groups of 3,3',3'',3'''- or 4,4',4'',4'''- positions. All prepared polymers, compounds, and phthalocyaninatocopper(II)-grafted polymers were characterized by FTIR. The sizing measurements were carried out in 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) compounds with and without grafting polymers. The results showed that the grafting process led to decreasing in particle size and increasing in surface area. The grafting process was reflected positively on the thermal degradation of 3,3',3'',3'''- (NH2)4PcCu(II) and 4,4',4'',4'''- (NH2)4PcCu(II) grafted polymers. They had higher thermal stability accompanied with higher char residue and T50% weight loss with 3,3',3'',3'''-(NH2)4PcCu(II) and their grafted polymers being the best.

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