scholarly journals Synthesis of 4-(2H-[1,2,4]-Triazol-5-ylsulfanyl)-1,2-dihydropyrazol-3-one via Ring-Switching Hydrazinolysis of 5-Ethoxymethylidenethiazolo [3,2-b][1,2,4]triazol-6-one

Molbank ◽  
10.3390/m1022 ◽  
2018 ◽  
Vol 2018 (4) ◽  
pp. M1022 ◽  
Author(s):  
Serhii Holota ◽  
Yaroslav Shylych ◽  
Halyna Derkach ◽  
Olexandr Karpenko ◽  
Andrzej Gzella ◽  
...  
Keyword(s):  
Acetic Anhydride ◽  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Chloroacetic Acid ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray ◽  
Ethanol Medium ◽  
Williamson Reaction

4-(1H-[1,2,4]-Triazol-5-ylsulfanyl)-1,2-dihydropyrazol-3-one (4) was synthesized with a yield of 55% via ring-switching hydrazinolysis of 5-ethoxymethylidenethiazolo[3,2-b][1,2,4] triazol-6-one (3) in ethanol medium. The initial 1H-[1,2,4]-triazole-3-thiol (1) was modified via a two-step reaction: S-alkylation with chloroacetic acid under Williamson reaction conditions, and further one-pot cyclization–condensation with triethylorthoformate in the acetic anhydride medium, yielding compound 3. The structures of compounds 3 and 4 were confirmed by LC-MS, NMR spectra and a single X-ray diffraction analysis (for compound 4).

Replacing sulfonate by carboxylate: application of pyridyliminocarboxylato copper(II) complexes in rac-lactide polymerization and Chan–Evans–Lam coupling

2019 ◽  
Vol 97 (3) ◽  
pp. 178-190 ◽  
Author(s):  
Valérie Hardouin Duparc ◽  
Clémentine Dimeck ◽  
Frank Schaper
Keyword(s):  
Molecular Sieves ◽  
Weight Control ◽  
Phenylboronic Acid ◽  
Side Reactions ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray ◽  
Induction Periods ◽  
Lactide Polymerization

Copper(II) complexes carrying pyridylmethyleneaminobenzoate or –propanoate ligands, LCuX, were prepared in one-pot reactions from pyridinecarboxaldehyde, aminobenzoic acid or β-alanine, and CuX2 (X = Cl, NO3, OAc, or OTf). All complexes were characterized by single-crystal X-ray diffraction studies and formed either dimers, tetramers, or coordination polymers. Attempted preparation of the respective alkoxide complexes, LCu(OR), was unsuccessful, but use of LCuX/NaOMe mixtures in rac-lactide polymerization indicated under some conditions coordination–insertion polymerization via a copper alkoxide as the mechanism. The complexes performed poorly in rac-lactide polymerization, showing low activities (12 h to completion at 140 °C), low to moderate heterotacticity (Pr = 0.6–0.8), and poor polymer molecular weight control (intramolecular transesterification). They were competent catalysts for Chan–Evans–Lam couplings with phenylboronic acid, without any indication of side reactions such as deboration or aryl homocoupling. The complexes were active in undried methanol, without addition of base, ligand, or molecular sieves. Aniline, n-octylamine, and cyclohexylamine were coupled quantitatively under identical reaction conditions. There is only little influence of the anion on activities (less than a factor of 2) but a strong influence on induction periods. The complexes were not active in CEL coupling with alcohols, phenols, or alkylboronic acids.

Synthesis of Nanosized Pseudoboehmite and γ-Al2O3 by Control Precipitation Method

2013 ◽  
Vol 684 ◽  
pp. 46-52 ◽  
Author(s):  
Zhou Qing Jiang ◽  
Hong Wen Ma ◽  
Jing Yang ◽  
Le Wang
Keyword(s):  
Aqueous Solution ◽  
Diffraction Analysis ◽  
Sodium Sulfate ◽  
Ageing Time ◽  
Precipitation Method ◽  
Al2o3 Nanoparticles ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray

Nanosized pseudoboehmite particles were synthesized by the precipitation of sodium sulfate and ammonia in aqueous solution at 70°C. After calcinations, the pseudoboehmite could successfully transfer to γ-Al2O3 nanoparticles while retaining their previous morphology. The influence of the reaction conditions on formation of pseudoboehmite and γ-Al2O3 had been researched in detail. The X-ray diffraction analysis showed that nanosized crystalline pseudoboehmite was formed at pH 8-8.5 after ageing 2 hours. Utilization of surfactant(PEG1000) would produce finer nanoparticles with well-dispersion. With the ageing time or the surfactant amount increasing, the morphology of the resulting particles transformed from spherical to fibrous

Two Zr−based heterometal−organic frameworks for efficient CO2 reduction under visible light

CrystEngComm ◽  
2021 ◽  
Author(s):  
Ying Wang ◽  
Yao-mei Fu ◽  
Si-qi You ◽  
xuexin Li ◽  
Xinlong Wang ◽  
...  
Keyword(s):  
Transition Metal ◽  
Visible Light ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Co2 Reduction ◽  
X Ray Diffraction ◽  
Transition Metal Cations ◽  
One Pot ◽  
X Ray ◽  
Secondary Building Units

Two new zirconium−based heterometal−organic frameworks, Zr3CP3−Mn (1) and Zr3CP3−Ni (2) constructed from [Cp3Zr3(μ3−O)(μ2−OH)3(IN)3] secondary building units and transition metal cations, were successfully synthesized through one−pot method. Single-crystal X-ray diffraction analysis...

scholarly journals Acetylation of Eugenol on Functionalized Mesoporous Aluminosilicates Synthesized from Amazonian Flint Kaolin

Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 478 ◽  
Author(s):  
Alex de Nazaré de Oliveira ◽  
Erika Tallyta Leite Lima ◽  
Eloisa Helena de Aguiar Andrade ◽  
José Roberto Zamian ◽  
Geraldo Narciso da Rocha Filho ◽  
...  
Keyword(s):  
Acetic Anhydride ◽  
Textural Properties ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Mesoporous Catalyst ◽  
Reaction Conditions ◽  
Alternative Source ◽  
X Ray ◽  
Acidic Sites ◽  
Catalyst Temperature

The present work was aimed to investigate the catalytic activity of a mesoporous catalyst synthesized from 3-mercaptopropyltrimethoxysilane (MPTS) functionalized Amazonian flint kaolin in the acetylation of eugenol with acetic anhydride. Materials were characterized by thermogravimetry (TGA), N2 adsorption (BET), X-ray dispersive energy spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and acid-base titration. The results presented proved the efficiency of flint kaolin as an alternative source in the preparation of mesoporous materials, since the material exhibited textural properties (specific surface area of 1071 m2 g−1, pore volume of 1.05 cm3 g−1 and pore diameter of 3.85 nm) and structural properties (d100 = 4.35 nm, a0 = 5.06 nm and Wt = 1.21 nm) within the required and characteristic material standards. The catalyst with the total amount of acidic sites of 4.89 mmol H+ g−1 was efficient in converting 99.9% of eugenol (eugenol to acetic anhydride molar ratio of 1:5, 2% catalyst, temperature and reaction time 80 °C and 40 min reaction). In addition, the reused catalyst could be successfully recycled with 92% conversion activity under identical reaction conditions.

Komplexbildung von Rhodium mit 6.6-Dimethylfulven / Complex Formation of Rhodium with 6.6-Dimethylfulvene

1983 ◽  
Vol 38 (11) ◽  
pp. 1454-1459 ◽  
Author(s):  
Jörn Müller ◽  
Rainer Stock ◽  
Joachim Pickardt
Keyword(s):  
Complex Formation ◽  
Diffraction Analysis ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray

Abstract Reaction of [(nbd)RhCl]2 (nbd = nor bornadiene) with CH3Li and 6.6-dimethylfulvene yields (nbd)Rh(2-propenylcyclopentadienyl). (cod)Rh(Cl)P(CH3)3 (cod = 1.5-cyclooctadiene), obtained by cleavage of [(cod)RhCl]2 with P(CH3)3, reacts with 6.6-dimethyl-fulvene and CH3Li or i-C3H7MgBr with substitution of cod by dimeric fulvene ligands the nature of which depends on the alkyl reagent. The new complexes were characterized by NMR spectra and in one case by X-ray diffraction analysis.

Degradation-insertion reactions of decaborane(14) with inorganic salts

1983 ◽  
Vol 48 (9) ◽  
pp. 2593-2603 ◽  
Author(s):  
Karel Baše
Keyword(s):  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Inorganic Salts ◽  
Analogous Reaction ◽  
X Ray Diffraction ◽  
Insertion Reactions ◽  
X Ray ◽  
Lewis Bases ◽  
H Nmr

Decaborane(14) reacts with NaNO2 in tetrahydrofuran forming the [9-tetrahydrofuran-6-NO2B10H12]- salt which after protonization with concentrated H2SO4 or diluted HCl affords azaboranes 6-NB9H12 and 4-NB8H13, respectively. The 6-NB9H12 azaborane is hydrolyzed to the 4-NB8H13 azaborane and reacts with Lewis bases under the formation of the 9-L-6-NB9H12 ligand derivatives (L = (CH)S, CHCN, (CH)P). By the reduction of 9-CHCN-6-NBH with LiAlH4 in tetrahydrofuran the 6-NB9H13- anion was prepared. By an analogous reaction of decaborane(14) with KHSO3 in water and by a subsequent protonization of the formed intermediate with concentrated H2SO4 or diluted HCl the thiaboranes 6-SB9H11 and 4-SB8H12, respectively, were prepared. The reaction of decaborane(14) with Na2SeO3 in tetrahydrofuran followed by the protonization of the intermediate with diluted HCl afforded the 7,8-Se2B9H9 species. Structures of all compounds were proposed on the basis of the 11B and 1H NMR spectra; in the case of 4-NB8H13, the structure was determined by the X-ray diffraction analysis.

Synthesis of Unsymmetrical Aza[7]helicenes by One-Pot Wittig–Heck and Photodehydrogenation Sequence

Synlett ◽  
2017 ◽  
Vol 28 (17) ◽  
pp. 2262-2266 ◽  
Author(s):  
Ashutosh Bedekar ◽  
Blessy Rajan
Keyword(s):  
Fluorescence Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Stepwise Procedure

An efficient protocol for the synthesis of unsymmetrical aza[7]helicenes has been developed. The bis-styryl-type substrates for regiospecific photodehydrogenative oxidative double cyclization to give helicenes were prepared by a one-pot Wittig–Heck sequence as well as a stepwise procedure. The derivatives were characterized by single-crystal X-ray diffraction analysis and fluorescence spectroscopy.

Electronic Structure of 2,6-Bis{.N-(2-hydroxyphenyl)immoinethyl}-4-methylphenol

1999 ◽  
Vol 54 (7) ◽  
pp. 929-939 ◽  
Author(s):  
Miki Hasegawa ◽  
Yasunori Yamada ◽  
Ken-ichi Kumagai ◽  
Toshihiko Hoshi
Keyword(s):  
Diffraction Analysis ◽  
Electronic Absorption ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
Mo Calculations ◽  
Absorption Bands ◽  
Polar Solvents ◽  
Additional Band ◽  
X Ray ◽  
H Nmr

The electronic and molecular structure of 2,6-bis{N-(2-hydroxyphenyl)iminomethyl}-4- methylphenol (hpimp) is clarified from the measurements of electronic absorption and 1H NMR spectra in various solvents and an X-ray diffraction analysis, together with MO calculations. Electronic absorption bands of hpimp are at 422, 397.9, 359, 341, 294.3, 265.8, and 224 nm in the non-polar solvent cyclohexane. In polar solvents, such as methanol, an additional band which is assigned to a partly formed keto-amine hpimp, is observed at 499 nm. From the 1H NMR spectra it is seen that hpimp exists in the enol-imine form in non-polar solvents, and as an equilibrium mixture of enol-imine and keto-amine forms in polar solvents. Each electronic absorption band of solid hpimp in a KBr disk is broadened compared with the solution state, and an additional band, again assigned to the keto-amine form, appears around 499 nm. An X-ray diffraction analysis shows that hpimp assumes a keto-amine structure in the solid state, and forms a column structure along the c-axis. MO calculations suggest that the enol-imine hpimp has a twist structure around the two C−C single bonds, the twist angle being 100° to 120°.

Structural organization of mercury(II) and copper(II) dithiocarbamates from EPR and 13C and 15N MAS NMR spectra and X-ray diffraction analysis

2008 ◽  
Vol 34 (1) ◽  
pp. 59-69 ◽  
Author(s):  
A. V. Ivanov ◽  
E. V. Korneeva ◽  
B. V. Bukvetskii ◽  
A. S. Goryan ◽  
O. N. Antzutkin ◽  
...  
Keyword(s):  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Structural Organization ◽  
Mas Nmr ◽  
X Ray Diffraction ◽  
X Ray

A Simple, One-Pot Synthesis of Trans-Substituted Spiro [5,5] undecane-1,5,9-triones with Aromatic Aldehydes and Meldrum's Acid as the Starting Materials

2015 ◽  
Vol 68 (10) ◽  
pp. 1599 ◽  
Author(s):  
Jingping Ou-Yang ◽  
Yu Zhao ◽  
Huailei Jiang ◽  
Lingxin Meng ◽  
Xingshu Li ◽  
...  
Keyword(s):  
1H Nmr ◽  
Aromatic Aldehydes ◽  
Quantum Mechanical ◽  
Quantum Mechanical Calculations ◽  
Meldrum's Acid ◽  
X Ray Diffraction ◽  
Meldrum’S Acid ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray

A simple, one-pot process for the construction of substituted spiro[5,5]undecane-1,5,9-triones using aromatic aldehydes and Meldrum’s acid, and aniline as a catalyst, is reported. Fifteen compounds were synthesized, and the trans/cis ratios were calculated based on 1H NMR analyses of the unpurified products. Quantum mechanical calculations and X-ray diffraction were undertaken to identify the configuration of compound 2a. The proposed mechanisms for these reactions are presented in this paper. In contrast to previous literature, this method endows excellent diastereoselectivity to a series of trans-substituted derivatives. The method is characterized by its simple operation, commercial availability of all materials, mild reaction conditions and moderate-to-good chemical yields.

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