Preparation of (mono)sulfonates: Suitable precursors for unnatural sulfonolipids

2021 ◽  
Vol 20 (2) ◽  
pp. 103-118
Author(s):  
Panayiotis V. Ioannou ◽  
Gerasimos M. Tsivgoulis
Keyword(s):  
Aqueous Solutions ◽  
1H Nmr ◽  
The Novel ◽  
Sulfonic Acids ◽  
Strecker Reaction ◽  
Relative Nucleophilicity

Aiming at the preparation of the novel unnatural, non-isosteric sulfonolipids bearing one, two and three acyl groups 8, 9 and 10, their precursors hydroxyl-containing sulfonates have been prepared from a variety of hydroxyl-containing halogenides and epoxides using the Strecker reaction. Thus, the sulfonates 16 and 22 were prepared pure, while the sulfonate 27 could only be prepared as a by-product using 1,4-dibromo-2,3-butanediol 26 and in low yields. For these reactions, probable pathways leading to the isolated or spectroscopically identified products are proposed. Conclusions about the relative nucleophilicity of SO32- compared to AsO33 - (as well as HO- which is present in their aqueous solutions) were drawn based on the yields of the corresponding arsonic acids and sodium sulfonates. The IR (KBr) and 1H NMR (D2O) spectra of sulfonates (and in some cases of their sulfonic acids) are analyzed and discussed.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

Facile Synthetic Protocols for the preparation of New Impurities in Pemetrexed Disodium Heptahydrate as an Anti-Cancer Drug

2021 ◽  
Vol 18 ◽  
Author(s):  
Rama Mohana Reddy Jaggavarapu ◽  
Venkatanarayana Muvvala ◽  
Ghojala Venkatareddy ◽  
Ravi Kumar Cheedarala
Keyword(s):  
Quality Control ◽  
Spectral Analysis ◽  
1H Nmr ◽  
Structure Elucidation ◽  
Research Work ◽  
Synthetic Methods ◽  
Cancer Drug ◽  
The Novel ◽  
Anti Cancer ◽  
Pemetrexed Disodium

: A facile synthetic protocols were employed to prepare process-related impurities associated with the synthesis of pemetrexed disodium heptahydrate, Alimta. The research work is described for the development of the novel synthetic methods and their structure elucidation of Pemetrexed glutamide, N-methyl pemetrexed, and N-methyl pemetrexed glutamide impurities. The listed impurities were deduced through spectral analysis such as 1H-NMR, 13CNMR, and HRMS. The target compounds can be used as the reference substances for the quality control.

γ-Radiolysis of disulfides in aqueous solution. III. L-Cysteine-D-penicillamine mixed disulfide

1969 ◽  
Vol 47 (6) ◽  
pp. 1037-1043 ◽  
Author(s):  
J. W. Purdie
Keyword(s):  
Aqueous Solution ◽  
Free Radicals ◽  
Aqueous Solutions ◽  
Dose Rate ◽  
Sulfonic Acids ◽  
Rate Dependent ◽  
Mixed Disulfide ◽  
Γ Rays ◽  
Symmetrical Disulfides ◽  
Symmetrical Disulfide

L-Cysteine-D-penicillamine mixed disulfide (CySSPen) was irradiated in aerated and deaerated aqueous solutions with 60Co γ-rays. G values were determined for all products identified after exposure to 10 000 rads. The major products were the sulfinic and sulfonic acids (CySO2H, CySO3H, and PenSO2H), the sulfhydryl derivatives (CySH and PenSH), symmetrical disulfides (CySSCy and PenSSPen), three trisulfides (CySSSCy, CySSSPen, and PenSSSPen), and ammonia. Each half of the disulfide behaved in exactly the same way as the corresponding symmetrical disulfide. Products from the CyS— part of the disulfide were dose rate dependent while products from the PenS— part were independent of dose rate. The reactions proposed for the symmetrical disulfides were adequate to explain radiolysis of the unsymmetrical disulfide.Radiolysis of a mixture of cystine and penicillamine disulfide was examined for comparison with the unsymmetrical disulfide and was found to give very similar results. It was concluded that the free radicals produced from the water attack each half at approximately equal rates.

1H NMR Spectroscopic Investigations on the Micellization and Gelation of PEO−PPO−PEO Block Copolymers in Aqueous Solutions

Langmuir ◽  
2007 ◽  
Vol 23 (19) ◽  
pp. 9596-9605 ◽  
Author(s):  
Jun-he Ma ◽  
Chen Guo ◽  
Ya-lin Tang ◽  
Hui-zhou Liu
Keyword(s):  
Block Copolymers ◽  
Aqueous Solutions ◽  
1H Nmr ◽  
Spectroscopic Investigations

scholarly journals A facile synthesis, dynamic 1H NMR and theoretical study the novel stable heterocyclic phosphorus ylides containing tetrazole

ARKIVOC ◽  
2009 ◽  
Vol 2008 (17) ◽  
pp. 173-183
Author(s):  
M. Amin Kazemian ◽  
Mahmoud Nassiri ◽  
Ali Ebrahimi ◽  
M. Taher Maghsoodlou ◽  
S. Mostafa Habibi-Khorassani ◽  
...  
Keyword(s):  
1H Nmr ◽  
Theoretical Study ◽  
The Novel ◽  
Phosphorus Ylides ◽  
Facile Synthesis ◽  
Dynamic 1H Nmr

scholarly journals Preparation of ferrocene core dendrimers and immobilization of AChE for detection of diclofop-methyl herbicide

2019 ◽  
Vol 38 (2) ◽  
pp. 215 ◽  
Author(s):  
Nurdan Kurnaz Yetim ◽  
Nurşen Sari
Keyword(s):  
Magnetic Susceptibility ◽  
1H Nmr ◽  
Substrate Concentration ◽  
Storage Stability ◽  
Molar Conductivity ◽  
Acetylcholine Esterase ◽  
The Novel ◽  
Optimal Parameters ◽  
Repeated Use ◽  
Inhibition Reaction

The aim of this work was to investigate diclofop-methyl detection (found in a variety of herbicides) using novel dendrimers that have ferrocene cores, as well as their Pt(II) and Pt(IV) complexes. Novel dendrimer structures were synthesized and characterized by molar conductivity, magnetic susceptibility, FTIR, UV-Vis, 1H-NMR and LC-MS methods. Then, the AChE (acetylcholine esterase) enzyme was immobilized on the novel dendrimers, and the optimal parameters (pH, temperature, repeated use, storage stability, substrate concentration) were determined for immobilized AChE. Lastly, changes in absorbance intensity were measured, and calibration graphs were plotted that reflect the inhibition reaction of immobilized AChE with diclofop-methyl. The inhibition interaction of the enzyme immobilized to the Pt(II) ion containing dendrimers was higher than that of the Pt(IV) ion containing dendrimers.

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