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91.
Giovanna Bruni Ines Ghione Vittorio Berbenni Andrea Cardini Doretta Capsoni Alessandro Girella Chiara Milanese Amedeo Marini 《Molecules (Basel, Switzerland)》2021,26(11)
The present work is a concrete example of how physico-chemical studies, if performed in depth, are crucial to understand the behavior of pharmaceutical solids and constitute a solid basis for the control of the reproducibility of the industrial batches. In particular, a deep study of the thermal behavior of glipizide, a hypoglycemic drug, was carried out with the aim of clarifying whether the recognition of its polymorphic forms can really be done on the basis of the endothermic peak that the literature studies attribute to the melting of the compound. A number of analytical techniques were used: thermal techniques (DSC, TGA), X-ray powder diffraction (XRPD), FT-IR spectroscopy and scanning electron microscopy (SEM). Great attention was paid to the experimental design and to the interpretation of the combined results obtained by all these techniques. We proved that the attribution of the endothermic peak shown by glipizide to its melting was actually wrong. The DSC peak is no doubt triggered by a decomposition process that involves gas evolution (cyclohexanamine and carbon dioxide) and formation of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which remains as decomposition residue. Thermal treatments properly designed and the combined use of DSC with FT-IR and XRPD led to identifying a new polymorphic form of 5-methyl-N-[2-(4-sulphamoylphenyl) ethyl] pyrazine-2-carboxamide, which is obtained by crystallization from the melt. Hence, our results put into evidence that the check of the polymorphic form of glipizide cannot be based on the temperature values of the DSC peak, since such a peak is due to a decomposition process whose Tonset value is strongly affected by the particle size. Kinetic studies of the decomposition process show the high stability of solid glipizide at room temperature. 相似文献
92.
A substituted donor–acceptor cyclobutenecarboxamide is synthesized with modest enantiocontrol through a chiral copper(I) complex catalyzed [3 + 1]-cycloaddition reaction of α-acyl diphenylsulfur ylides with 3-siloxy-2-diazo-3-butenamides. With a methyl substituent on the 4-position of the 3-butenamide, the cis-vicinal-3,4-disubstituted cyclobutenecarboxamide is formed with >20:1 diastereocontrol. Donor-acceptor 3-methyl-2-siloxycyclopropenecarboxamide is rapidly formed from the reactant enoldiazoamide and undergoes catalytic ring opening to give only the Z-γ-substituted metallo-enolcarbene. Elimination from 3-siloxy-2-diazo-3-pentenamide to form the conjugated 3-siloxy-2,4-pentadienamide is competitive but minimized at low temperature. 相似文献
93.
Yttrium(III) Nitrate: A Powerful Catalyst for Green and Rapid Synthesis of Some Supramolecules 下载免费PDF全文
A convenient and rapid procedure for the synthesis of calix[4]resorcinarenes as useful supramolecules has been developed via a reaction of aryl aldehydes with resorcinol in the presence of yttrium(III) nitrate under solvent‐free conditions. This eco‐friendly method has many appealing attributes such as excellent yields, short reactions times, and simple work‐up procedures. 相似文献
94.
Two 2,6‐Dioxabicyclo[3.3.1]nonan‐3‐ones from Phragmanthera capitata (Spreng.) Balle (Loranthaceae) 下载免费PDF全文
Bruno N. Lenta Joél T. Ateba Jean R. Chouna Makoah N. Aminake Flore Nardella Gabriele Pradel Beate Neumann Hans Georg Stammler Catherine Vonthron‐Sénécheau Silvère Ngouela Norbert Sewald 《Helvetica chimica acta》2015,98(7):945-952
Phytochemical investigation of the leaves of Phragmanthera capitata collected on Cassia spectabilis tree led to the isolation of two natural lactones, rel‐(1R,5S,7S)‐7‐[2‐(4‐hydroxyphenyl)ethyl]‐2,6‐dioxabicyclo[3.3.1]nonan‐3‐one ( 1 ) and 4‐{2‐[rel‐(1R,3R,5S)‐7‐oxo‐2,6‐dioxabicyclo[3.3.1]non‐3‐yl]ethyl}phenyl 3,4,5‐trihydroxybenzoate ( 2 ) together with the known compounds betulinic acid ( 3 ), dodoneine ( 4 ), quercetin 3‐O‐α‐L ‐rhamnopyranoside ( 5 ), quercetin 3‐O‐α‐L ‐arabinofuranoside ( 6 ), quercetin ( 7 ), betulin ( 8 ), lupeol ( 9 ), and sitosterol ( 10 ). Their structures were established by means of modern spectroscopic techniques, and the relative configuration of compound 1 was confirmed by X‐ray analysis. Compounds 1 and 2 were tested in vitro for their antiplasmodial activity against the Plasmodium falciparum chloroquine sensitive‐strains NF54 and 3D7. Compound 2 exhibited good antiplasmodial activity against both strains with IC50 of 2.4 and 4.9 μM , respectively, while compound 1 was inactive. 相似文献
95.
Synthesis of 5‐Cyano‐2‐Carbethoxythieno[2,3‐b]thiophenyl‐3,4‐Diisothiocyanates and Its Utility IN Heterocyclic Synthesis under Phase Transfer Catalytic Technique 下载免费PDF全文
O. A. Abd Allah 《中国化学会会志》2015,62(11):991-999
Regarding to the importance of thieno[2,3‐b]thiophens and isothiocyanaetes reactiveties in the physical, chemical and pharmaceutical fields, this study has been undertaken to prepare the target compound 5‐cyano‐2‐carbethoxythieno[2,3‐b]thiophenyl‐3,4‐diisothiocyanates via a safe method. The formed isothiocyanates derivative was reacted with aromatic amines, acid hydrazied and some active methylene groups, followed by cyclization reaction for the formed intermediates to give new series of heterocyclic compounds 相似文献
96.
The Identification of a Novel Highly Condensed Pentacyclic Heteroaromatic Ring System 1,3,5,5b,6,8,10,10b‐Octaazacyclopenta[h,i]Aceanthrylene and its Application in the Synthesis of 5,7‐Substituted Pyrazolo[4,3‐d]Pyrimidines 下载免费PDF全文
Libor Havlíček Daniela Moravcová Vladimír Kryštof Miroslav Strnad 《Journal of heterocyclic chemistry》2015,52(3):669-673
Pyrazolo[4,3‐d]pyrimidines are of interest as potential kinase inhibitors. This article describes the formation of a novel highly conjugated, condensed, centrosymmetric heteroaromatic compound, 4,9‐dichloro‐2,7‐diisopropyl‐1,3,5,5b,6,8,10,10b‐octaazacyclopenta[h,i]aceanthrylene ( 3 ), during the chlorination of 5,7‐dihydroxypyrazolo[4,3‐d]pyrimidine ( 1 ) with phenylphosphonic dichloride. The nucleophilic attack of benzylamine on 3 afforded N‐benzyl‐5‐chloro‐3‐isopropyl‐1H‐pyrazolo[4,3‐d]pyrimidin‐7‐amine ( 6 ), which was further substituted to yield a pyrazolo[4,3‐d]pyrimidine analogue of roscovitine, a well‐known cyclin‐dependent kinase inhibitor. 相似文献
97.
Yuan Yang Ming‐Bo Zhou Xuan‐Hui Ouyang Rui Pi Ren‐Jie Song Jin‐Heng Li 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2015,127(22):6695-6699
A rhodium(III)‐catalyzed [3+2]/[5+2] annulation of 4‐aryl 1‐tosyl‐1,2,3‐triazoles with internal alkynes is presented. This transformation provides straightforward access to indeno[1,7‐cd]azepine architectures through a sequence involving the formation of a rhodium(III) azavinyl carbene, dual C(sp2) H functionalization, and [3+2]/[5+2] annulation. 相似文献
98.
[DBU‐H]+ and H2o as effective catalyst form for 2,3‐dihydropyrido[2,3‐d]pyrimidin‐4(1H)‐ones: A DFT Study 下载免费PDF全文
DFT investigations are carried out to explore the effective catalyst forms of DBU and H2O and the mechanism for the formation of 2,3‐dihydropyrido[2,3‐d]‐pyrimidin‐4(1H)‐ones. Three main pathways are disclosed under unassisted, water‐catalyzed, DBU and water cocatalyzed conditions, which involves concerted nucleophilic addition and H‐transfer, concerted intramolecular cyclization and H‐transfer, and Dimroth rearrangement to form the product. The results indicated that the DBU and water cocatalyzed pathway is the most favored one as compared to the rest two pathways. The water donates one H to DBU and accepts H from 2‐amino‐nicotinonitrile ( 1 ), forming [DBU‐H]+‐H2O as effective catalyst form in the proton migration transition state rather than [DBU‐H]+‐OH?. The hydrogen bond between [DBU‐H]+···H2O··· 1 ? decreases the activation barrier of the rate‐determining step. Our calculated results open a new insight for the green catalyst model of DBU‐H2O. © 2015 Wiley Periodicals, Inc. 相似文献
99.
100.
采用稳态和瞬态荧光法对2-(2-羟苯基)苯并噻唑(HBT)与七元瓜环(CB7)的超分子作用及CB7分子纳米腔限制作用对HBT激发态质子转移(ESIPT)过程进行了研究,并采用Benesi-Hildebrand方程对荧光数据进行处理,以确定超分子复合物的组成比.结果表明,在N,N-二甲基甲酰胺(DMF)和二氯甲烷溶液中,CB7与HBT的作用均形成化学计量比为1∶1的主客体复合物,HBT的质子转移对溶剂很敏感,CB7的加入,使HBT的荧光寿命降低,量子产率增大.在DMF溶液中,CB7的加入促进了酚氧负离子的形成,而在二氯甲烷溶液中,CB7的加入限制了HBT的激发态质子转移.结构优化计算表明,CB7与HBT能形成化学计量比为1∶1的复合物. 相似文献