One-pot approach to synthesize hyperbranched poly(thiol–ether amine) (hPtEA) through sequential “thiol–ene” and “epoxy–amine” click reactions

2015 ◽  
Vol 6 (39) ◽  
pp. 6946-6954 ◽  
Author(s):  
Jing Yu ◽  
Zhilong Su ◽  
Hongjie Xu ◽  
Xiaodong Ma ◽  
Jie Yin ◽  
...  

We demonstrated a one-pot approach to synthesize hyperbranched poly(thiol–ether amine) (hPtEA) through sequential “thiol–ene” and “epoxy–amine” click reactions, both of which were well traced using in situ1H-NMR spectra.

2018 ◽  
Vol 14 ◽  
pp. 3011-3017
Author(s):  
Akın Sağırlı ◽  
Yaşar Dürüst
Keyword(s):  
2D Nmr ◽  
X Ray ◽  
H Nmr ◽  
Tof Ms ◽  

The present work describes an unfamiliar reaction of 5-(chloromethyl)-3-substituted-phenyl-1,2,4-oxadiazoles with KCN affording trisubstituted 1,2,4-oxadiazol-5-ylacetonitriles and their parent alkanes, namely, 1,2,3-trisubstituted-1,2,4-oxadiazol-5-ylpropanes. To the best of our knowledge, the current synthetic route leading to decyanated products will be the first in terms of a decyanation process which allows the transformation of trisubstituted acetonitriles into alkanes by the incorporation of KCN with the association of in situ-formed HCN and most likely through the extrusion of cyanogen which could not be detected or isolated. In addition, the plausible mechanisms were proposed for both transformations. The structures of the title compounds were identified by means of IR, 1H NMR, 13C NMR, 2D NMR spectra, TOF–MS and X-ray measurements.


1998 ◽  
Vol 10 (3) ◽  
pp. 217-229 ◽  
Author(s):  
Hans R Kricheldorf ◽  
Oliver Bolender ◽  
Thomas Wollheim

A new trifunctional monomer was prepared from ethyl-4-(4,5-dichlorophthalimido) benzoate and 4-mercaptophenol. The phenolic OH groups were acetylated, and the carboxylic group was silylated to reduce the melting temperature. A successful homopolycondensation yielding a completely soluble hyperbranched poly(ester-imide) was only obtained when the silylated monomer was used. This branching monomer was polycondensed with a difunctional imide monomer to yield co(polyester-imide)s having a variable degree of branching. Furthermore, copolycondensations with 3-acetoxybenzoic acid or 3,5-bisacetoxybenzoic acid (and their trimethylsilyl esters) were studied. The composition of the resulting copolyesters were checked by elemental analyses and 1H NMR spectra. The glass transition temperatures ( T g s) showed a systematic variation between the values of the parent homopolyesters.


2006 ◽  
Vol 61 (9) ◽  
pp. 1162-1165 ◽  
Author(s):  
Ali S. Mahasneh

Abstract A direct one pot, three-component nitro-Mannich reaction of a nonenolizable aldehyde, aniline or one of its ring-substituted derivatives and nitromethane was carried out on silica gel surface. The products of the reaction, 2-aminonitroethane, were obtained in high yields. IR, 1H NMR, 13C NMR spectra and elemental analysis confirmed the structures of the products.


1980 ◽  
Vol 45 (10) ◽  
pp. 2695-2699 ◽  
Author(s):  
Jiří Křepelka ◽  
Jiří Holubek ◽  
Miroslav Semonský

Chloride of 4,4-bis(4-ethylphenyl)-2,3-dibromo-2-butenoic acid (VII), prepared in situ, reacted with aliphatic alcohols and benzyl alcohol with the formation of esters II-VI. Reaction of the chloride VII with aromatic alcohols gave 7-ethyl-4-(4'-ethylphenyl)-2,3-dibromo-1-naphthol (VIII), whose structure was corroborated by IR and 1H NMR spectra. Compounds II-VI and VIII exhibited weaker antineoplastic effects than Edikron (I).


2020 ◽  
Vol 17 ◽  
Author(s):  
Rajiv Kumar Tonk ◽  
Vivek Yadav ◽  
Mohsin Hasan

: In recent years substitution at the third position on phthalides has been proven a valuable synthetic intermediate for the development of active molecules. We reported a direct and efficient one-pot method for the synthesis of 3-aryl Phthalides performed by the addition of organo-zinc reagent on methyl-2-formylbenzoate; reagent formed in-situ by the reaction between diethylzinc and different aryl boronic acid derivatives without using any kind of ligand. The possible mechanism involved a coordinated zinc carbonyl transition state, arylation, and followed by the intramolecular cyclization. The substituents groups in boronic having different electronic and steric properties played an important role in the reaction completion time and yield. The structure elucidation and confirmation of the synthesized compounds were done by using H-NMR analytical data. The method can be useful for the synthesis of various scaffolds and intermediates in the search of potentially active compounds.


2014 ◽  
Vol 10 ◽  
pp. 2671-2676 ◽  
Author(s):  
Chao Wang ◽  
Yan-Hong Jiang ◽  
Chao-Guo Yan

The one-pot four-component reaction of benzohydrazide (2-picolinohydrazide), acetylenedicarboxylate, isatins and malononitrile (ethyl cyanoacetate) with triethylamine as base catalyst afforded functionalized 1-benzamidospiro[indoline-3,4'-pyridines] in good yields. 1H NMR spectra indicated that an equilibrium of cis/trans-conformations exist in the obtained products.


2020 ◽  
Vol 24 (8) ◽  
pp. 900-908
Author(s):  
Ram Naresh Yadav ◽  
Amrendra K Singh ◽  
Bimal Banik

Numerous O (oxa)- and S (thia)-glycosyl esters and their analogous glycosyl acids have been accomplished through stereoselective glycosylation of various peracetylated bromo sugar with benzyl glycolate using InBr3 as a glycosyl promotor followed by in situ hydrogenolysis of resulting glycosyl ester. A tandem glycosylating and hydrogenolytic activity of InBr3 has been successfully investigated in a one-pot procedure. The resulting synthetically valuable and virtually unexplored class of β-CMGL (glycosyl acids) could serve as an excellent potential chiral auxiliary in the asymmetric synthesis of a wide range of enantiomerically pure medicinally prevalent β-lactams and other bioactive molecules of diverse medicinal interest.


1981 ◽  
Vol 46 (8) ◽  
pp. 1913-1929 ◽  
Author(s):  
Bohdan Schneider ◽  
Pavel Sedláček ◽  
Jan Štokr ◽  
Danica Doskočilová ◽  
Jan Lövy

It was found that three crystalline forms of ethylene glycol dibenzoate can be prepared. Infrared and Raman spectra of these three forms, as well as of the glassy and liquid states, were measured. From 3JHH coupling constants obtained by analysis of the 13C satellite band of the -CH2- group in 1H NMR spectra, and from the 3JCH coupling constants of the -CO.O.CH2- fragment obtained by analysis of the carbonyl band in 13C NMR spectra it was found that in the liquid state the -CH2-CH2- group exists predominantly in the gauche conformational structure, and the bonds C-O-C-C assume predominantly a trans orientation. The results of the analysis of NMR and vibrational spectra were used for the structural interpretation of conformationally sensitive bands in vibrational spectra of ethylene glycol dibenzoate.


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