Tartrate Salt Research Articles

Influence of Protective Colloids on Calcium Tartrate Stability and the Astringency Perception in a Red Wine.

Calcium tartrate instability in wines has been a neglected topic for many years. However, it seems that this problem is gaining prominence, and the industry welcomes inputs to address this issue. Among the alternatives that winemakers use for tartrate salt stabilization, the addition of authorized protective colloids is one of the best choices because they are easy to apply and have a low energetic cost. In the present study, the same red wine was treated with five different commercially available protective colloids in triplicate. The effectiveness of such colloids on calcium tartrate potential instability was estimated, in addition to their side effects on the phenolic composition of the treated wines and their astringency perception, as assessed by sensory analyses of the treated wine. The results show that, under these trial conditions, carboxymethylcellulose is the best choice for reducing the risk of calcium tartrate precipitation in wine. Moreover, the application of protective colloids to the wines had little effect on their color, phenolic composition, or evolution during one year of bottle storage. Finally, the addition of protective colloids did not impact the astringency intensity, but it influenced the dynamic perception of astringency according to the temporal dominance of sensation analysis.

Use of differential scanning calorimetry as a rapid, effective in-process check method for impurity quantitation of an early clinical batch of Giredestrant (GDC-9545)

Giredestrant (GDC-9545) is a selective estrogen receptor degrader (SERD) that was developed for treatment of ER+/HER2− metastatic breast cancer. An anhydrous crystalline tartrate salt was identified as the solid form suitable for clinical development. An early clinical batch of the active pharmaceutical ingredient (API)/drug substance failed to pass the GMP purity specifications owing to the presence of a substantial amount of high molecular weight impurities (oligomers), as determined by size exclusion chromatography. Several trial rework batches were manufactured using various re-slurry and recrystallization conditions to purge impurities in the drug substance to adhere to purity specifications. Based on the melting point depression of the API in presence of oligomers in these rework batches, a differential scanning calorimetry method was developed to quantify impurity content as a function of melting point onset of the API. This thermal analysis method was used as a surrogate for chromatography as a rapid, effective in-process check method for impurity quantitation to enable the timely release of the final reworked clinical batch. Post release, the % w/w oligomer value determined by calorimetry was in excellent agreement to that obtained by size exclusion chromatography.

Ammonium and Tartrate Salts as Alternatives to Neutral Aqueous Electrolytes for Supercapacitors

AbstractSupercapacitors are promising energy storage devices in terms of power density and lifetime. Organic electrolytes are frequently applied in commercial supercapacitor devices. However, their water‐based counterparts are much safer, more sustainable and cost‐effective. In this study we therefore present, for the first time, aqueous tartrate‐based electrolytes (sodium tartrate / ammonium tartrate) for supercapacitor applications, and relate them to well‐known inorganic aqueous electrolytes like Na2SO4. Additionally, the influence of the cation on the electrochemical performance of supercapacitors is investigated using sodium and ammonium cations for comparison. We demonstrate the electrochemical performance and physicochemical properties of ammonium tartrate / sulfate and sodium tartrate / sulfate. An improvement of the conductivity in the range of 40–60 % was achieved by the exchange of sodium cation with ammonium cation. Carbon electrodes in newly introduced aqueous tartrate‐based electrolytes deliver high specific capacitances up to 117 Fg−1. Furthermore, electrical double layer capacitors (EDLCs) containing 1 M ammonium tartrate display a high energy density at 0.1 Ag−1 and at 10 Ag−1 (9.88 Whkg−1 and 1.14 Whkg−1, respectively). Floating tests show excellent long‐term performance. Tartrate‐based EDLCs retain >80 % of their initial capacitance at 1.6 V cell voltage (120 h floating time). In the case of ammonium tartrate electrolyte, a novel metal‐free and non‐toxic concept for an eco‐friendly supercapacitor device is proposed.

Synthesis and Resolution of an Axially Chiral Spirocyclic Quaternary Ammonium Ion‐Based Phase‐Transfer Catalyst

AbstractWe report the synthesis of a novel spirocyclic quaternary ammonium salt that possesses axial chirality. Enantiopure material was obtained by fractional crystallization of the corresponding (R,R)‐tartrate salt. Application of this chiral quaternary ammonium salt in phase‐transfer catalytic asymmetric alkylation of glycinate Schiff base was examined.

Synthesis, Characterization, and Stability Assessment for the Benzoate, Hydrochloride, Malonate, and Nicotinate Salts of Bedaquiline.

Bedaquiline has been approved as a combination therapy to treat multi-drug-resistant tuberculosis in adults ≥ 18 years old. The citrate, fumarate, phosphate, and tartrate salts have obtained patents, but the structures for these moieties have not been extensively described in the literature; only the powder X-ray patterns have been published. To expand the knowledge of the bedaquiline structure, this study provides detailed information for the synthesis, elucidation, characterization, and stability of four additional new potential molecular entities, namely, benzoate, hydrochloride (HCl), nicotinate, and malonate salts. The salts were formed using a 1:1 ratio of the counter ions (acids) to a 30 mg equivalent of the bedaquiline free base. The principles of the International Conference on Harmonization Q6 were used to characterize the new salts and their stability-indicating parameters were evaluated at 0, 3, and 6 months under accelerated conditions of 40 °C and 75% relative humidity. The benzoate salt exhibited the lowest tendency to lose its chemical potency. Aside from the HCl salt, the others retained their chemical structure, displaying long-term stability. All salts were non-hygroscopic and the hydrated benzoate and nicotinate salts were stable to dehydration. Regarding their chemical potencies, thermal analysis, chemical stability, and water sorption potential, the salts were ranked as follows: benzoate > malonate > nicotinate > HCl.

Se with Se-C bonds encapsulated in a honeycomb 3D porous carbon as an excellent performance cathode for Li-Se batteries

Li-Se batteries have risen to prominence as promising lithium-ion batteries thanks to their ultrahigh volumetric energy density and the high electrical conductivity of Se. However, the use of Li-Se batteries is limited not only by the large volume expansion and dissolution of polyselenides in the cathodes during cycling, but also the low selenium loading. A highly effective and currently feasible approach to simultaneously tackle these problems is to position the selenium in a carbon matrix with a sufficient pore volume to accommodate the expansion while increasing the interfacial interaction between the selenium and carbon. We have synthesized a novel cathode material (Se@HPC) for Li-Se batteries of a honeycomb 3D porous carbon derived from a tartrate salt, that was impregnated with Se to produce Se-C bonds. The pore volume of the honeycomb 3D porous carbon was as high as 1.794 cm3 g−1, which allowed 65 wt% selenium to be uniformly encapsulated. Moreover, the strong chemical bonds between selenium and carbon stabilize the selenium, thus inhibiting its huge volume expansion and the dissolution of polyselenides, and promoting charge transfer during cycling. As expected, a Se@HCP cathode has excellent cyclability and a good rate performance. After 200 cycles at 0.2 C, its specific capacity remains at 561 mA h g−1, 83% of the theoretical value, and decays by only 0.058% per cycle. It also has a large capacity of 472.8 mA h g−1 under a high current density of 5 C.

Ionic strength and buffering capacity of emulsifying salts determine denaturation and gelation temperatures of whey proteins

Ionic conditions affect the denaturation and gelling of whey proteins, affecting the physical properties of foods in which proteins are used as ingredients. We comprehensively investigated the effect of the presence of commonly used emulsifying salts on the denaturation and gelling properties of concentrated solutions of β-lactoglobulin (β-LG) and whey protein isolate (WPI). The denaturation temperature in water was 73.5°C [coefficient of variation (CV) 0.49%], 71.8°C (CV 0.38%), and 69.9°C (CV 0.41%) for β-LG (14% wt/wt), β-LG (30% wt/wt), and WPI (30% wt/wt), respectively. Increasing the concentration of salts, except for sodium hexametaphosphate, resulted in a linear increase in the denaturation temperature of WPI (kosmotropic behavior) and an acceleration in its gelling rate. Sodium chloride and tartrate salts exhibited the strongest effect in protecting WPI against thermal denaturation. Despite the constant initial pH of all solutions, salts having buffering capacity (e.g., phosphate and citrate salts) prevented a decrease in pH as the temperature increased above 70°C, resulting in a decline in denaturation temperature at low salt concentrations (≤0.2 mol/g). When pH was kept constant at denaturation temperature, all salts except sodium hexametaphosphate, which exhibited chaotropic behavior, exhibited similar effects on denaturation temperature. At low salt concentration, gelation was the controlling step, occurring up to 10°C above denaturation temperature. At high salt concentration (>3% wt/wt), thermal denaturation was the controlling step, with gelation occurring immediately after. These results indicate that the ionic and buffering properties of salts added to milk will determine the native versus denatured state and gelation of whey proteins in systems subjected to high temperature, short time processing (72°C for 15 s).

Crystallization of Mn(II) and Cd(II) Complexes in A Water-Methanol System: Tartrate vs Nicotinamide Ligand Selectivity

Ligand selectivity of tartrate vs nicotinamide in a water-methanol system has been observed in the crystallization of Mn(II) and Cd(II) complexes. These complexes were crystallized at room temperature by a layered solution technique using a water-methanol mixture solvent in a M(II):tartrate:nicotinamide (M = Mn, Cd) molar ratio of 1:1:2. Complexes of M(II)-nicotinamide and M(II)-tartrate were also prepared for data comparison. Analysis of the crystals by infrared spectroscopy, powder-X-ray diffraction and qualitative anion test showed that in a presence of both tartrate and nicotinamide, the Mn(II) forms neutral Mn(II)-tartrate hydrate complex, whereas the Cd(II) forms ionic Cd(II)-nicotinamide chloride complex. In the case of Mn(II) complex, tartrate tend to coordinate as ligand than the nicotinamide, although molar ratio of nicotinamide was doubled than that of tartrate ligand. In contrast, the neutral nicotinamide ligand is more predominant to coordinate in the Cd(II) complex than the anionic tartrate. The tartrate-nicotinamide ligand selectivity in the crystallization of Mn(II) and Cd(II) complexes is likely due to the use of tartrate salt as precursor and the choice of solvent mixture. In addition, powder-XRD analysis confirms that there was no indication of M(II)-tartrate and M(II)-nicotinamide that co-crystallized together at the same time by both metal ions.

Galvanostatic optimization of polyaniline coating on mild steel in tartrate medium for corrosion protection

Optimization of polyaniline (PANI) coating on mild steel (MS) surface has been studied in 0.3 M aniline + 0.2 M sodium potassium tartrate (Na-K Tartrate) by galvanostatic polarization. The current densities of 0.5, 0.75. 1 and 2 mA cm-2 are used for the electrodeposition of PANI on MS. The obtained PANI coatings have been characterized for its morphology using an optical microscope and corrosion performance by using potentiodynamic polarization in 0.4 M Na2SO3 solution simulating an industrial environment. The results reveal a sequential process of dissolution of MS, passivation of MS by forming tartrate salt followed by oxidation of aniline monomer and subsequential nucleation and growth of PANI coating. It is found that the PANI coating obtained at 0.5 mA cm-2 results in better coating producing corrosion inhibition efficiency (IE) of approximately 90% compared to IE of about 75% for coating obtained at 2 mA cm-2.

Salts and Polymorph Screens for Bedaquiline

Bedaquiline is used to treat multi-resistant tuberculosis in adults. The fumarate salt is commercially available and used in the product Sirturo. To provide open access to bedaquiline molecule once the patent on the chemical substance expires, new salts were screened. This work offers additional information on the bedaquiline system, as new salts may present better pharmacokinetic properties. The current studies focus on the attempted isolation of the acetate, benzoate, benzenesulfonate, hydrobromide, succinate, hydrochloride, tartrate, lactate, maleate, malate, and mesylate salts of bedaquiline. Potential salts were screened using a unique combination of conventional screening, and small-scale experiments supplemented by crystallographic analysis and infrared microspectroscopy. Salts were prepared on a larger scale by dissolving 1:1 ratios of the individual salt formers and bedaquiline base (30 mg, 0.055 mmol) in different solvents and allowing the solutions to evaporate or crystallize. X-ray diffraction (XRD) techniques and spectroscopic and thermal analyses were employed to characterize the salts. The benzoate and maleate salts were selected as lead candidates after reviewing preliminary characterization data. To determine the most stable forms for the leads, a polymorph screen was conducted using solvents of various polarities. These salt screens successfully generated five new salts of bedaquiline, namely, benzoate, maleate, hydrochloride, besylate, and mesylate. The existence of these salts was confirmed by powder XRD, proton NMR, and IR spectroscopies. TGA and DSC thermal analysis along with hot-stage optical microscopy were further used to characterize the salts. The polymorph screen conducted on the salts suggested the absence of additional polymorphs at 1 g scale.

Activation of Neuronal Nicotinic Receptors Inhibits Acetylcholine Release in the Neuromuscular Junction by Increasing Ca2+ Flux through Cav1 Channels.

Cholinergic neurotransmission is a key signal pathway in the peripheral nervous system and in several branches of the central nervous system. Despite the fact that it has been studied extensively for a long period of time, some aspects of its regulation still have not yet been established. One is the relationship between the nicotine-induced autoregulation of acetylcholine (ACh) release with changes in the concentration of presynaptic calcium levels. The mouse neuromuscular junction of m. Levator Auris Longus was chosen as the model of the cholinergic synapse. ACh release was assessed by electrophysiological methods. Changes in calcium transients were recorded using a calcium-sensitive dye. Nicotine hydrogen tartrate salt application (10 μM) decreased the amount of evoked ACh release, while the calcium transient increased in the motor nerve terminal. Both of these effects of nicotine were abolished by the neuronal ACh receptor antagonist dihydro-beta-erythroidine and Cav1 blockers, verapamil, and nitrendipine. These data allow us to suggest that neuronal nicotinic ACh receptor activation decreases the number of ACh quanta released by boosting calcium influx through Cav1 channels.

Abstract 1248: ERGi-USU-6 salt derivatives, a selective inhibitor for ERG positive prostate cancer cells

Abstract Background: Approximately half of prostate cancer patients harbor the oncogenic TMPRSS2-ERG gene fusion expressing the ERG oncoprotein. Our lead compound, ERGi-USU, is a potent small molecule inhibitor that binds the atypical kinase RIOK2 leading to the inhibition of the growth of ERG positive cancer cells reducing ERG levels. We have developed a new and more effective derivative, ERGi-USU-6. We have reported the new salts formula EB3P0-16 of ERGi-USU-6 inhibiting the growth of ERG positive prostate cancer cells at IC50=89nM achieving the range of FDA approved drugs. Encouraged by this success we have designed and tested a broad array of new salt formulations to further improve the biological activity of ERGi-USU-6. Methods: From fifty potential salt formulations, we prioritized candidate salts based on the structure, solubility, ionic hydrophobic/hydrophilic characteristics. Series of salts were synthesized by chemical reactions with ERGI-USU-6. Selected formulas include, bisulfate, butyrate, carbonate, salicylate, tartrate salts. The different stages of salt formulation included the testing of a) preformulation, b) pre-formulation processing, c) physicochemical properties, d) solubility, e) pKa, f) partition coefficient, g) pH- solubility profiling, h) prodrug formulation, and i) polymorphism. The IC50 values for ERG protein inhibition was compared to the parental compound and were calculated in a 12-step dilution range and were repeated thrice. The protein levels were quantified by measuring protein levels in a wide range using iBright instrument. Results: A total of 21 salt formulas were prioritized and synthesized. The result confirmed the lead characteristics of EB3P0-16. However, among the new formulas four other salt derivatives showed improved ERG protein inhibition compared to the parental compound. Also, we gained new insights in designing the next generation of formula by the exclusion of chemical structures that did not lead to improvement. Conclusion: This study confirmed EB3P0-16 as the lead formula of ERGi-USU-6. We found four new salt formulas with improved activity achieving ERG protein inhibition within the effective concentration range. The significance of our findings opens the possibility of new deigns towards the pre-clinical testing of ERG inhibitors. Disclaimer: The opinions or assertions contained herein are the private ones of the author/speaker and are not to be construed as official or reflecting the views of the Department of Defense, the Uniformed Services University of the Health Sciences or any other agency of the U.S. Government. The identification of specific products, scientific instrumentation, or organization is considered an integral part of the scientific endeavor and does not constitute endorsement or implied endorsement on the part of the author, DoD, or any component agency. Citation Format: Binil Eldhose, Charles P. Xavier, Mallesh Pandrala, Albert Dobi, Sanjay V. Malhotra. ERGi-USU-6 salt derivatives, a selective inhibitor for ERG positive prostate cancer cells [abstract]. In: Proceedings of the American Association for Cancer Research Annual Meeting 2021; 2021 Apr 10-15 and May 17-21. Philadelphia (PA): AACR; Cancer Res 2021;81(13_Suppl):Abstract nr 1248.

Development of industrial efficient asymmetric synthesis of endothelin-A antagonist ABT-546: A case study based on green chemistry perspective

The catalytic, extremely effective enantioselective conjugate-addition strategy was approved by via 4 mol% of bis(oxazoline)-Mg(OTf)2 along with amine complex as co-catalyst. The magnicium triflate based catalysis afford 88% selectivity in the molecule and provide less dependence on the tartrate salt for enantioselectivity, which was previously prepared for attaining chiral purity for the synthesis of the endothelin-A antagonist ABT-546. Along with enantioselective conjugate-addition the new strategy involves green solvents in the final steps of ABT-546 drug preparation. The use of green solvent owes its own advantage of minimizing the residues remaining in the API synthesized. The article includes the case study of the ABT-546 to discuss the green chemistry objectives fulfilled by pharma industry.

Acoustic, thermal and optical properties of organic based disodium tartrate salt

In this work, acoustic, thermal, and optical properties were tested on the different concentrations of the Disodium Tartrate solutions. First, the viscosity studies were analyzed for the Disodium tartrate in the concentration range from 2% to 20% with different temperatures 303K, 308K, 313K, and 318K. It was noted that the relative viscosity and the activation energy of the prepared compound increase with increases in concentration and decreases with temperature increases. The properties like density and ultrasonic velocity are varied when increases the concentration of the aqueous solutions of Disodium Tartrate. In this study, the values of adiabatic compressibility show an inverse behavior when compared with ultrasonic velocity due to the interaction between solute and solvent molecules. Also observed that the inter-molecular free length is maximum for a lower percentage. The free volume for the compound is maximum at 2% and a minimum of 20%, since it reduces when the internal pressure increases. It was revealed that the classical absorption coefficient and relaxation time for Disodium Tartrate is minimum for lower percentage and minimum for a higher percentage. The interactions between the solute and solvent are confirmed through the property like specific Acoustical impedance. It was noted that the increase in internal pressure increases the concentration of the compound. The ion-solvent interaction was discussed by the relative association study, thus the values of relative association increases with an increase in concentration. The Rao’s and Wada’s constant increases linearly in aqueous solutions of Disodium Tartrate for the entire system.

Salt Engineering of Aripiprazole with Polycarboxylic Acids to Improve Physicochemical Properties.

Aripiprazole (APZ) has poor physicochemical properties and bitter taste. The current study aimed to prepare salts of APZ with polycarboxylic acids (citric, malic, and tartaric acids) to improve physicochemical properties and impart sour taste to the drug. The salts were prepared by solubilization-crystallization method, and characterized by electron microscopic, spectroscopic, diffractometry, and thermal methods. The salts were assessed for pH solubility, pH-stability, dissolution, and solid-state stability. Fourier transformed infrared, X-ray powder diffraction, and differential scanning calorimetry data indicated formation of new solid phases. APZ and the salts exhibited pH-dependent solubility. The pH solubility curve shape was inverted "V," inverted "W," and inverted "U" for APZ, APZ-Citrate, and APZ-Malate and APZ-Tartrate, respectively. Compared to APZ, the solubility of salts at pH4, 5, and 6 was 3.6-7.1, 23.9-31.5, and 143.4-373.3 folds of APZ. Increase in solubility in water by citrate, malate, and tartrate salts was 5562.8, 21,284.7, and 22,846.7 folds of APZ. The salt formation also leads to an increase in rate and extent of dissolution. The dissolution extent was 3.5 ± 0.5, 71.3 ± 1.2, 80.1 ± 6.2, and 86.1 ± 1.1% for APZ, APZ-Citrate, APZ-Malate, and APZ-Tartrate, respectively. Liquid and solid-state stabilities of the salts were comparable to APZ. In conclusion, salts of APZ with polycarboxylic acids improved solubility, and dissolution, and impart sour taste, which may improve palatability of the drug.

Fifteen 4-(2-meth-oxy-phen-yl)piperazin-1-ium salts containing organic anions: supra-molecular assembly in zero, one, two and three dimensions.

Fifteen 4-(2-meth-oxy-phen-yl)piperazin-1-ium salts containing organic anions have been prepared and structurally characterized. In the isostructural 4-chloro-benzoate and 4-bromo-benzoate salts, C11H17N2O+·C7H4ClO2 - (I) and C11H17N2O+·C7H4BrO2 - (II), and the 4-iodo-benzoate salt C11H17N2O+·C7H4IO2 - (III), the ions are linked by N-H⋯O hydrogen bonds, forming centrosymmetric R 4 4(12) four-ion aggregates; a similar aggregate is formed in the 2-chloro-benzoate salt (V), isomeric with (I). In the 2-fluoro-benzoate salt C11H17N2O+·C7H4FO2 - (IV), and the isomorphous pair of salts, the 2-bromo-benzoate (VI), isomeric with (II) and 2-iodo-benzoate (VII), isomeric with (III), N-H⋯O and C-H⋯π(arene) interactions link the components into three-dimensional arrays. Four-ion R 4 4(12) aggregates are also found in the 2-methyl-benzoate, 4-amino-benzoate and 4-nitro-benzoate salts, C11H17N2O+·C8H7O2 - (VIII), C11H17N2O+·C7H6NO2 - (IX) and C11H17N2O+·C7H4NO4 - (X), but those in (IX) are linked into complex sheets by an additional N-H⋯O hydrogen bond. In the 3,5-dinitrobenzoate salt, C11H17N2O+·C7H3N2O6 -·2H2O (XI), N-H⋯O and O-H⋯O hydrogen bonds link the components into a complex ribbon structure. In the picrate salt, C11H17N2O+·C6H2N3O7 - (XII), the four-ion aggregates are linked into chains of rings by C-H⋯O hydrogen bonds. In the hydrogen maleate salt, C11H17N2O+·C4H3O4 - (XIII), two- and three-centre hydrogen bonds link the ions into a ribbon structure while both anions contain very short but asymmetric O-H⋯O hydrogen bonds, having O⋯O distances of 2.4447 (16) and 2.4707 (17) Å. O-H⋯O Hydrogen bonds link the anions in the hydrogen fumarate salt (XIV), isomeric with (XIII), into chains that are linked into sheets via N-H⋯O hydrogen bonds. In the hydrogen (2R,3R)-tartrate salt, C11H17N2O+·C4H5O6 -·1.698H2O (XV), the anions are linked into sheets by O-H⋯O hydrogen bonds. Comparisons are made with the structures of some related compounds.

Protection of Wine from Protein Haze Using Schizosaccharomyces japonicus Polysaccharides.

Nowadays commercial preparations of yeast polysaccharides (PSs), in particular mannoproteins, are widely used for wine colloidal and tartrate salt stabilization. In this context, the industry has developed different processes for the isolation and purification of PSs from the cell wall of Saccharomyces cerevisiae. This yeast releases limited amounts of mannoproteins in the growth medium, thus making their direct isolation from the culture broth not economically feasible. On the contrary, Schizosaccharomyces japonicus, a non-Saccharomyces yeast isolated from wine, releases significant amounts of PSs during the alcoholic fermentation. In the present work, PSs released by Sch. japonicus were recovered from the growth medium by ultrafiltration and their impact on the wine colloidal stability was evaluated. Interestingly, these PSs contribute positively to the wine protein stability. The visible haziness of the heat-treated wine decreases as the concentration of added PSs increases. Gel electrophoresis results of the haze and of the supernatant after the heat stability test are consistent with the turbidity measurements. Moreover, particle size distributions of the heat-treated wines, as obtained by Dynamic Light Scattering (DLS), show a reduction in the average dimension of the protein aggregates as the concentration of added PSs increases.

Study on a Three-Step Rapid Assembly of Zolpidem and Its Fluorinated Analogues Employing Microwave-Assisted Chemistry.

We developed an efficient microwave-assisted three-step synthesis of zolpidem and its fluorinated analogues 1–3. The procedure relays on the utilization of easily accessible and inexpensive starting materials. Our protocol shows superior performance in terms of yield and purity of products, compared to conventional heating systems. Notably, the total time needed for reaction accomplishment is significantly lower comparing to oil bath heating systems. Finally, we have performed a detailed study on the preparation of zolpidem tartrate salt I, and we assessed its particle-sizes using a polarizing microscope. Our goal was to select the appropriate method that generates the acceptable particle-size, since the solid-size directly influences solubility in biological fluids and further bioavailability. We believe that the disclosed procedure will help to produce a lab-scale quantity of zolpidem and its fluorinated derivatives 1–3, as well as zolpidem tartrate salt I, with suitable fine-particle size for further biological experimentation.

Synthesis of a crosslinked poly(ionic liquid) and evaluation of its antimony binding properties

First ever ionic liquid derived sorbent for antimony was synthesised. The charged functional groups of the polymer showed preferential binding and strong affinity for difficult to remove anionic species of antimony. The sorbent was synthesised by crosslinking co-polymerisation of 1-butyl-3-vinylimidazolium bromide with N,N-methylenebis(acrylamide). SEM-EDS analysis showed that the polymer retained the bromide counter ions. Antimony removal properties under wide solution conditions, including the presence of competitor ions, were investigated. Maximum antimony binding and selectivity was at pH 3.0. Variation in saturation capacity with respect to the crosslinker amount matched with the calculated capacity values. Maximum uptake obtained was 4.6 and 3.2 mmol/g for Sb(III) and Sb(V) respectively. Tartrate salt of Sb(III) showed better binding through the interaction of tartrate with the imidazole moieties of the polymer. In less than 15 min, saturation capacity was achieved for Sb(III), while over 90% of uptake was complete for Sb(V). Investigations on sorption mechanism, which included synthesis and comparative evaluation of the non-ionic counterpart polyvinylimidazole as sorbent, indicated the uptake to be through anion exchange. Sb(III) specific binding against Sb(V) was seen in the presence of nitrilotriacetic acid.

Stereoselective Synthesis for Potential Isomers of Ticagrelor Key Starting Material

Tartrate salt of carbocyclic amine 2 is one of the key starting materials for the synthesis of Ticagrelor 1. During the synthesis of 1, the isomers of 2 also need to be considered as potential impurities and characterized before establishing the specification of product. In the present work, detailed study has been carried out to synthesize the related substances of 2, and their structure characterization has been discussed.