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Pinelopi Voulgari Dimitrios Alivertis Konstantinos Skobridis 《Helvetica chimica acta》2021,104(11):e2100066
Osimertinib, a third generation potent and specific EGFR inhibitor is an important drug against many forms of cancer. It was synthesized by an improved and highly efficient protocol, revisiting the classical synthetic process and modifying parameters, such as solvents, temperature, reagents, and reaction time. A cost-effective, environmentally friendly methodology for the synthesis of osimertinib was established, which gave shorter reaction times, saved labor by eliminating purification steps through column chromatography, and enhanced yields. Four of the seven steps in total, were proceeded quantitatively or almost quantitatively (ca. 98 %). This synthetic protocol provides a very high overall yield, up to 68 %. In addition, the entire approach enables the preparation of osimertinib analogues and could be extended in the synthesis of other structurally similar bioactive compounds. 相似文献
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It has been proved that the electrolysis parameters strongly influence the structural properties of nickel electrodeposits,
mainly the crystalline growth, preferred orientation and surface morphology. To determine the structural characteristics of
nickel and composite nickel matrix electrocoatings, prepared under either direct current or pulse current conditions, the
electron microscopy techniques have proved very important tools. In particular, investigation of the distribution and percentage
of microparticles incorporated in the metallic matrix during preparation of nickel composite electrocoatings demands the use
of techniques such as energy dispersion spectroscopy (EDS) or image analysis. 相似文献
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Manuel Cordova Pinelopi Moutzouri Bruno Simões de Almeida Daria Torodii Prof. Lyndon Emsley 《Angewandte Chemie (International ed. in English)》2023,62(8):e202216607
The resolution of proton solid-state NMR spectra is usually limited by broadening arising from dipolar interactions between spins. Magic-angle spinning alleviates this broadening by inducing coherent averaging. However, even the highest spinning rates experimentally accessible today are not able to completely remove dipolar interactions. Here, we introduce a deep learning approach to determine pure isotropic proton spectra from a two-dimensional set of magic-angle spinning spectra acquired at different spinning rates. Applying the model to 8 organic solids yields high-resolution 1H solid-state NMR spectra with isotropic linewidths in the 50–400 Hz range. 相似文献
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Pinelopi C. Ioannou Evriklia S. Lianidou Dimitrios G. Konstantianos 《Analytica chimica acta》1995,300(1-3):237-241
A very simple, rapid and highly sensitive fluorimetric method for the determination of diflunisal in serum and urine is described. The method is based on the formation of a ternary complex between diflunisal, Tb3+ and EDTA in alkaline aqueous solutions. This complex exhibits very intense terbium ion luminescence with a main emission maximum at 546 nm when excited at 284 nm. Optimum conditions for the complex formation have been investigated. The detection limit for diflunisal is 2.4 μg 1−1, while the range of application is 0.01–6.00 mg 1−1. The method has been successfully applied for the determination of diflunisal in untreated human serum and urine samples. Analytical recoveries from serum and urine samples spiked with diflunisal were in the ranges of 96.8–101.2% and 98.0–102.0%, respectively. 相似文献
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Dr. Pinelopi Moutzouri Dr. Federico M. Paruzzo Bruno Simões de Almeida Dr. Gabriele Stevanato Prof. Lyndon Emsley 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2020,132(15):6294-6297
The typical linewidths of 1H NMR spectra of powdered organic solids at 111 kHz magic-angle spinning (MAS) are of the order of a few hundred Hz. While this is remarkable in comparison to the tens of kHz observed in spectra of static samples, it is still the key limit to the use of 1H in solid-state NMR, especially for complex systems. Here, we demonstrate a novel strategy to further improve the spectral resolution. We show that the anti-z-COSY experiment can be used to reduce the residual line broadening of 1H NMR spectra of powdered organic solids. Results obtained with the anti-z-COSY sequence at 100 kHz MAS on thymol, β-AspAla, and strychnine show an improvement in resolution of up to a factor of two compared to conventional spectra acquired at the same spinning rate. 相似文献
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Pinelopi Moutzouri Manuel Cordova Bruno Simões de Almeida Daria Torodii Lyndon Emsley 《Angewandte Chemie (International ed. in English)》2023,62(21):e202301963
One key bottleneck of solid-state NMR spectroscopy is that 1H NMR spectra of organic solids are often very broad due to the presence of a strong network of dipolar couplings. We have recently suggested a new approach to tackle this problem. More specifically, we parametrically mapped errors leading to residual dipolar broadening into a second dimension and removed them in a correlation experiment. In this way pure isotropic proton (PIP) spectra were obtained that contain only isotropic shifts and provide the highest 1H NMR resolution available today in rigid solids. Here, using a deep-learning method, we extend the PIP approach to a second dimension, and for samples of L-tyrosine hydrochloride and ampicillin we obtain high resolution 1H-1H double-quantum/single-quantum dipolar correlation and spin-diffusion spectra with significantly higher resolution than the corresponding spectra at 100 kHz MAS, allowing the identification of previously overlapped isotropic correlation peaks. 相似文献
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Pinelopi Moutzouri Federico M. Paruzzo Bruno Simes de Almeida Gabriele Stevanato Lyndon Emsley 《Angewandte Chemie (International ed. in English)》2020,59(15):6235-6238
The typical linewidths of 1H NMR spectra of powdered organic solids at 111 kHz magic‐angle spinning (MAS) are of the order of a few hundred Hz. While this is remarkable in comparison to the tens of kHz observed in spectra of static samples, it is still the key limit to the use of 1H in solid‐state NMR, especially for complex systems. Here, we demonstrate a novel strategy to further improve the spectral resolution. We show that the anti‐z‐COSY experiment can be used to reduce the residual line broadening of 1H NMR spectra of powdered organic solids. Results obtained with the anti‐z‐COSY sequence at 100 kHz MAS on thymol, β‐AspAla, and strychnine show an improvement in resolution of up to a factor of two compared to conventional spectra acquired at the same spinning rate. 相似文献
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