scholarly journals Investigation of reaction conditions on synthesis of steroidal bromohydrin and structural analysis of novel 6α-brom-5β-hydroxy derivative

2018 ◽  
Vol 16 (2) ◽  
pp. 219-228
Author(s):  
Ivana Kuzminac ◽  
Olivera Klisuric ◽  
Andrea Nikolic ◽  
Marija Sakac
Keyword(s):  
Crystal Structure ◽  
Perchloric Acid ◽  
Crystal Structure Analysis ◽  
Hydroxy Derivative ◽  
Reaction Products ◽  
Reaction Conditions ◽  
X Ray ◽  
Hypobromous Acid ◽  
Series Of Experiments

Reaction conditions variation and its influence on the reaction of 3?- acetoxy-17-oxa-17a-homoandrost-5-en-16-one with in situ generated hypobromous acid was investigated. Hypobromous acid was generated from N-bromoacetamide or Nbromosuccinimide and perchloric acid, and as solvent dioxane, dimethoxyethane or tetrahydrofuran were used. After a series of experiments, it was determined that the number of the reaction products depends on the reagent used, solvents, perchloric acid concentration and the presence/absence of daylight. It has also been found that the yields of certain compounds depend also on the reaction time and temperature. 6?-Bromo-5?- hydroxy derivate is obtained by usage of NBA and 0.28 M perchloric acid in dioxane on daylight. Its structure was confirmed by NMR and X-ray crystal structure analysis.

1,3-Dipolar [3+3] Cycloaddition of 1,4-Benzodiazepinone-Based Nitrones with α-Halohydroxamates for Diastereoselective Synthesis of Novel d-Edge Heterocycle-Fused 1,4-Benzodiazepinones

Synlett ◽  
2021 ◽  
Author(s):  
Hong-Wu Zhao ◽  
Heng Zhang ◽  
Lu-Yu Cai ◽  
Zhe Tang ◽  
Xiao-Zu Fan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Reaction Mechanism ◽  
Single Crystal ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Diastereoselective Synthesis ◽  
Reaction Conditions ◽  
Relative Configuration ◽  
X Ray ◽  
Single Crystal Structure Analysis

Promoted by K2CO3 (2.0 equiv), the 1,3-dipolar [3+3] cycloaddition between 1, 4-benzodiazepinone-based nitrones and α-halohydroxamates processed smoothly under the mild reaction conditions and delivered structurally novel and complex cis or trans-configured d-edge-heterocycle-fused 1,4-benzodiazepinones in up to >99% isolated yield with >20:1 dr. The relative configuration of the title chemical entities was clearly identified with the use of X-ray single crystal structure analysis. The reaction mechanism was assumed to interpret the diastereoselective production of the obtained cis or trans-configured d-edge-heterocycle-fused 1, 4-benzodiazepinones.

scholarly journals A New Synthetic Route to (Trifluoromethyl)quinolines: Nickel-Catalyzed Insertion of an Alkyne into an Aromatic C–S Bond by Formation of a Thianickelacycle and Thermal Desulfidation

Synlett ◽  
2021 ◽  
Author(s):  
Takuya Kurahashi ◽  
Seijiro Matsubara ◽  
Tasuku Inami
Keyword(s):  
Crystal Structure ◽  
Fine Structure ◽  
Sulfur Atom ◽  
Crystal Structure Analysis ◽  
Insertion Reaction ◽  
Synthetic Route ◽  
X Ray ◽  
X Ray Absorption ◽  
Single Crystal Structure Analysis

AbstractWe have developed a nickel-catalyzed insertion reaction of an alkyne into a 2-(trifluoromethyl)-1,3-benzothiazole to give a seven-membered benzothiazepine that is converted into a 2-(trifluoromethyl)quinoline by thermal desulfidation. This process can be considered a formal substitution of a sulfur atom with an alkyne. The structure of the thianickelacycle intermediate formed through oxidative addition of a C–S bond in the benzothiazole to nickel(0) was confirmed by X-ray single-crystal structure analysis and in situ X-ray absorption fine-structure spectroscopy.

Unique molecular structure and properties of novel purple intermediates of phthalocyanine derivative

2003 ◽  
Vol 07 (01) ◽  
pp. 58-69 ◽  
Author(s):  
Fumiihiro Maeda ◽  
Kenjiro Uno ◽  
Kazuchika Ohta ◽  
Makiko Sugibayashi ◽  
Naotake Nakamura ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Metal Salt ◽  
Crystal Structure Analysis ◽  
Structure And Properties ◽  
Reaction Conditions ◽  
X Ray ◽  
Microwave Reactor ◽  
Single Crystal Structure Analysis

When long alkylthio-substituted phthalocyaninato copper(II) complexes, ( C n S )8 PcCu , were rapidly prepared in an α-diol by using our developed see-through microwave reactor and/or a conventional hot stirrer, novel purple intermediates were selectively obtained instead of the expected green complex, ( C n S )8 PcCu , for some specific combinations of the reaction solvent and metal salt. The reaction conditions to obtain the purple intermediates were established and the unique molecular structure was clarified for a buthylthio-substituted intermediate by X-ray single crystal structure analysis.

ChemInform Abstract: Thermolysis of Trifluoromethyl-Containing Vinyldiazocarbonyl Compounds and X-Ray Crystal Structure Analysis of Unexpected Reaction Products.

ChemInform ◽  
2014 ◽  
Vol 45 (15) ◽  
pp. no-no
Author(s):  
Valerij A. Nikolaev ◽  
Murat B. Supurgibekov ◽  
Ralf Haiges ◽  
Anthony Linden ◽  
G. K. Surya Prakash
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Reaction Products ◽  
X Ray ◽  
Unexpected Reaction

Thermolysis of trifluoromethyl-containing vinyldiazocarbonyl compounds and X-ray crystal structure analysis of unexpected reaction products

2013 ◽  
Vol 156 ◽  
pp. 322-326 ◽  
Author(s):  
Valerij A. Nikolaev ◽  
Murat B. Supurgibekov ◽  
Ralf Haiges ◽  
Anthony Linden ◽  
G.K. Surya Prakash
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Reaction Products ◽  
X Ray ◽  
Unexpected Reaction

scholarly journals In situhydrogen loading on zirconium powder

2015 ◽  
Vol 22 (4) ◽  
pp. 995-1000 ◽  
Author(s):  
Tuerdi Maimaitiyili ◽  
Jakob Blomqvist ◽  
Axel Steuwer ◽  
Christina Bjerkén ◽  
Olivier Zanellato ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Energy ◽  
Crystal Structure Analysis ◽  
X Ray ◽  
Commercially Pure ◽  
Pure Zirconium ◽  
First Time ◽  
Zirconium Powder ◽  
Hydride Phases

For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studiedin situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement.

scholarly journals Formation and structure of the first metal complexes comprising amidinoguanidinate ligands

2016 ◽  
Vol 72 (11) ◽  
pp. 1526-1531 ◽  
Author(s):  
Farid M. Sroor ◽  
Phil Liebing ◽  
Cristian G. Hrib ◽  
Daniel Gräsing ◽  
Liane Hilfert ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Metal Complexes ◽  
Solid State Reaction ◽  
The Novel ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray

The first metal complexes comprising amidinoguanidinate ligands have been prepared and structurally characterized, namely bis[μ-N,N′,N′′,N′′′-tetraisopropyl-1-(1-butylamidinato)guanidinato-κ3N1,N2:N2]bis[(tetrahydrofuran)lithium], [Li2(C18H37N4)2(C4H8O)2], (2), and [bis(tetrahydrofuran)lithium]-di-μ-chlorido-{(N,N′-dicyclohexyl-1-butylamidinato-κ2N1,N2)[N,N′,N′′,N′′′-tetracyclohexyl-1-(1-butylamidinato)guanidinato-κ2N1,N2]holmate(III)}, [HoLiCl2(C4H8O)2(C17H31N2)(C30H53N4)], (3). The novel lithium amidinoguanidinate precursors Li[nBuC(=NR)(NR)C(NR)2] [1:R= Cy (cyclohexyl),2:R=iPr) were obtained by treatment ofN,N′-diorganocarbodiimides,R—N=C=N—R(R=iPr, Cy), with 0.5 equivalents ofn-butyllithium under well-defined reaction conditions. An X-ray diffraction study of2revealed a ladder-type dimeric structure in the solid state. Reaction of anhydrous holmium(III) chloride within situ-prepared2afforded the unexpected holmium `ate' complex [nBuC(=NCy)(NCy)C(NCy)2]Ho[nBuC(NCy)2](μ-Cl)2Li(THF)2(3) in 71% yield. An X-ray crystal structure determination of3showed that this complex contains both an amidinate ligand and the new amidinoguanidinate ligand.

1,2-Deoxygenation of vic-Dihydroxyindenoimidazoles: Optimization of a Novel Deoxygenation Reagent

2004 ◽  
Vol 59 (10) ◽  
pp. 1143-1152 ◽  
Author(s):  
Hans-Jörg Hemmerling ◽  
Angelika Merschenz-Quack ◽  
Hartmut Wunderlich
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Reaction Conditions ◽  
X Ray ◽  
Mechanism Of The Reaction

Abstract Treatment of vic-dihydroxyindeno[1,2-d]imidazoles with N,N,N’,N’-tetraalkyl sulfurous diamides yields indeno[1,2-d]imidazoles by deoxygenation. Isochromeno[3,4-d]imidazoles are formed as byproducts. An X-ray crystal structure analysis confirmed the structure of deoxygenated products. The ratio of products depending on the reaction conditions was analyzed. A mechanism of the reaction is discussed.

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