• Title/Summary/Keyword: ‘One-pot’ synthesis

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Magnetic Nanoparticle Immobilized N-Propylsulfamic Acid as a Recyclable and Efficient Nanocatalyst for the Synthesis of 2H-indazolo[2,1-b]phthalazine-triones in Solvent-Free Conditions: Comparison with Sulfamic Acid

  • Rostami, Amin;Tahmasbi, Bahman;Yari, Ako
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1521-1524
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    • 2013
  • N-Propylsulfamic acid supported onto magnetic $Fe_3O_4$ nanoparticles (MNPs-PSA) was used as an efficient and magnetically recoverable catalyst for synthesis of 2H-Indazolo[2,1-b]phthalazine-1,6,11(13H)-trione derivatives from the three-component, one-pot condensation reaction of phthalhydrazide, aromatic aldehydes and cyclic 1,3-diones, in good to excellent yields at $100^{\circ}C$ under solvent-free conditions. The catalyst was easily separated with the assistance of an external magnetic field from the reaction mixture and reused for several consecutive runs without significant loss of its catalytic efficiency. In order to compare, the synthesis of 2H-Indazolo[ 2,1-b]phthalazine-1,6,11(13H)-trione derivatives in the presence of catalytic amount of sulfamic acid (SA) under same reaction condition was also reported.

Synthesis of Core@Shell-Structured Silicon@Carbon Nanoparticles by One-Pot Spray Pyrolysis Process and Application as Anode Materials for Lithium-Ion Batteries (단일 분무 열분해 공정을 이용한 코어@쉘 구조의 Si@C 나노 분말 합성 및 리튬 이온 전지 음극소재 적용)

  • Seong Ho Jung;Jae Seob Lee;Jung Sang Cho
    • Clean Technology
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    • v.30 no.3
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    • pp.220-227
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    • 2024
  • As the demand for lithium-ion batteries with high capacity and high energy density has rapidly increased, silicon anodes (theoretical capacity = 3,570 mA h g-1) have garnered attention as potential replacements for conventional graphite anodes (theoretical capacity = 372 mA h g-1). However, silicon anodes suffer from severe volume expansion (~360%) during lithiation, low ionic conductivity (10-14 ~ 10-13 cm2 S-1), and low electrical conductivity (10-2 S cm-1), resulting in poor cycling and rate performance. To address these issues, this study synthesized core@shell-structured silicon@carbon nanoparticles (Si@C NPs) via a one-pot spray pyrolysis process using Pluronic-F127. Pluronic-F127 in the spray solution contributes to the synthesis of nanoparticles by preventing the formation of silicon nanoparticle/dextrin agglomerates and by undergoing pyrolysis simultaneously. Additionally, dextrin derived amorphous carbon was coated on the surface of the silicon nanoparticles to act as an electron transport pathway within the anodes and enhance the electrical contact between the silicon nanoparticles. The Si@C NPs exhibited a discharge capacity of 1,912 mA h g-1 after 50 cycles at 1.0 A g-1 and high rate capabilities (discharge capacity of 1,493 mA h g-1 at 3.0 Ag-1). The silicon@carbon composite nanoparticle synthesis strategy based on the spray pyrolysis process presented in this study is expected to offer a new direction for improving the performance of silicon anode materials.

Application of Acrylic Resins Containing Acetoacetoxy Group and 80% Solid Contents to High-Solid Coatings (아세토아세톡시기 함유 80% 고형분인 아크릴수지의 하이솔리드 도료에의 적용)

  • Park, Hong-Soo;Hong, Seok-Young;Kim, Song-Hyoung;Yoo, Gyu-Yeol;Ahn, Sung-Hwan;Hahm, Hyun-Sik
    • Journal of the Korean Applied Science and Technology
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    • v.23 no.4
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    • pp.319-327
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    • 2006
  • In order to prepare high-solid coatings, first acrylic resins (HSAs) which contain 80% solid were synthesized, and then the prepared resins were cured with isocyanate at room temperature. In the synthesis of HSAs, viscosity, number average molecular weight $(M_n)$ and conversion were $1372{\sim}2700$ cps, $1520{\sim}1650$ and $83{\sim}87%$, respectively. Among the four kinds of initiators used, tert-amylperoxy-2-ethyl hexanoate was the most proper one in the synthesis of HSAs. With increasing $T_g$ values, viscosity increased rapidly and molecular weight increased slowly. As a result of the examination of coated films, it was found that $60^{\circ}$ specular gloss, impact resistance, heat resistance and cross-hatch adhesion were good, and pencil hardness, drying time and pot life were poor.

One Pot Synthesis of Substituted [1,2,4]-Triazolo [1',2':1,2]pyrimido [6,5-b]-quinoline and Its Antibacterial Activity

  • Joshi, Ratnadeep S.;Mandhane, Priyanka G.;Chate, Asha V.;Khan, Wajid;Gill, Charansingh H.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2341-2344
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    • 2010
  • A convenient synthesis of substituted [1,2,4]-triazolo [1',2':1,2]pyrimido[6,5-b]-quinoline 4(a-i) from substituted 2-chloroquinoline-3-carbaldehyde 1(a-i) and 4H-1,2,4-triazol-3-amine 2 by using $SiO_2/K_2CO_3$ under microwave irradiation. This method affords the [1,2,4]-Triazolo [1',2':1,2]pyrimido[6,5-b]-quinoline 4(a-i) under the influence of microwave irradiation in solvent-free conditions within short span (12 - 20 min), & gaves excellent yields (89 - 95%). All the synthesized compounds were further screened for their antibacterial activities. Some of our compounds showed excellent antibacterial activities against control drugs.

Three Component Solvent-free Synthesis of Chroman-2,4-dione-based Heterocyclic Ketene Aminal (HKA) Derivatives by "GAP" Chemistry

  • Yu, Fu-Chao;Hao, Xiao-Pan;Jiang, Xiu-Yang;Yan, Sheng-Jiao;Lin, Jun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1625-1632
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    • 2014
  • A concise and efficient one-pot synthesis of chroman-2,4-dione-based HKA derivatives by three component reaction of HKAs, triethoxymethane and 4-hydroxycoumarin derivatives under solvent-free and catalyst-free conditions is described. This protocol has many advantages, in that the GAP (Group-Assistant-Purification) chemistry process is involved in this method. As a result, the experimenter can avoid cumbersome process steps such as traditional chromatography and recrystallization purifications. The desired products can be easily obtained by washing the crude products with 95% EtOH.

Spirodiclofen Analogues as Potential Lipid Biosynthesis Inhibitors: A Convenient Synthesis, Biological Evaluation, and Structure-Activity Relationship

  • Ke, Shaoyong;Sun, Tingting;Zhang, Zhigang;Zhang, Ya-Ni;Liang, Ying;Wang, Kaimei;Yang, Ziwen
    • Bulletin of the Korean Chemical Society
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    • v.31 no.8
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    • pp.2315-2321
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    • 2010
  • Twenty spirodiclofen analogues have been designed and conveniently synthesized via three steps including esterification, one-pot heterocyclization, and acylation reactions. The target molecules have been identified on the basis of analytical spectra ($^1H$ NMR, $^{13}C$ NMR and ESI-MS) data. All newly synthesized compounds have been screened for their potential insecticidal and herbicidal activity by standard method. The preliminary assays indicated that some of analogues displayed moderate to good insecticidal activity against Plutella xylostella compared with spirodiclofen, and some compounds showed obvious activity against Brassica chinensis. Structure-activity relationship (SAR) is also discussed based on the experimental data.

Alumina Supported Ammonium Dihydrogenphosphate (NH4H2PO4/Al2O3): Preparation, Characterization and Its Application as Catalyst in the Synthesis of 1,2,4,5-Tetrasubstituted Imidazoles

  • Emrani, Anahita;Davoodnia, Abolghasem;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2385-2390
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    • 2011
  • Preparation of ammonium dihydrogenphosphate supported on alumina ($NH_4H_2PO_4/Al_2O_3$) and its primary application as a solid acid supported heterogeneous catalyst to the synthesis of 1,2,4,5-tetrasubstituted imidazoles by a one-pot, four-component condensation of benzil, aromatic aldehydes, primary amines, and ammonium acetate under thermal solvent-free conditions were described. The results showed that the novel catalyst has high activity and the desired products were obtained in high yields. Furthermore, the products could be separated simply from the catalyst, and the catalyst could be recycled and reused with only slight reduction in its catalytic activity. Characterization of the catalyst was performed by FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques.

Facile Synthesis of Dendritic Benzyl Chlorides from Their Alcohols with Methanesulfonyl Chloride/$Et_3N$ (덴드리틱 벤질 클로라이드의 효율적인 합성)

  • Lee, Jae-Wook;Han, Seung-Choul;Kim, Hee-Joo;Kim, Jung-Hwan;Lee, Un-Yup;Kim, Byoung-Ki;Sung, Sae-Reum;Kang, Hwa-Shin;Kim, Ji-Hyeon;Huh, Do-Sung
    • Polymer(Korea)
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    • v.31 no.5
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    • pp.417-421
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    • 2007
  • A successful rapid synthesis of dendritic benzyl chlorides from dendritic benzyl alcohols using methanesulfonyl chloride/$Et_3N$ as activating agents was described. In this method, each dendritic benzyl chloride can be prepared in one pot: no isolation of intermediate mesylated dendrons is required. The key steps in the syntheses of dendritic benzyl chlorides were the mesylation of the hydroxymethyl group followed by the chlorination by in-situ generated triethylammonium chloride.

One-pot synthesis of gold trisoctahedra with high-index facets

  • Kim, Do Youb;Choi, Kyeong Woo;Im, Sang Hyuk;Park, O Ok;Zhong, Xiao-Lan;Li, Zhi-Yuan
    • Advances in materials Research
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    • v.1 no.1
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    • pp.1-12
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    • 2012
  • There have been many efforts on the generating metal nanocrystals enclosed by high-index facets for the use as highly active catalysts. This paper describes a facile synthesis of Au trisoctahedra with high-index facets. In brief, the Au trisoctahdra were prepared by reduction of $HAuCl_4$ in N,N-dimethylformamide (DMF) containing poly (vinyl pyrrolidone) (PVP) and trace amount of $AgNO_3$. The Ag ions in the reaction solution played a critical role in controlling the trisoctahedral shape of the final product by underpotential deposition (UPD) on the Au surfaces. The as-prepared Au trisoctahedra were single crystal and enclosed by high-index {441}, {773} and {331} facets.

One-Pot Reaction Involving Two Different Amines and Formaldehyde Leading to the Formation of Poly(Macrocyclic) Cu(II) Complexes

  • Lee, Yun-Taek;Kang, Shin-Geol
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2517-2522
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    • 2012
  • New polynuclear poly(hexaaza macrocyclic) copper(II) complexes $[1](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, $[2](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, and $[3](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$ have been prepared by the one-pot reaction of formaldehyde with ethylenediamine and 1,2-bis(2-aminoethoxy)ethane, 1,3-diaminopropane, or 1,6-diaminohexane in the presence of the metal ion. The polymer complexes contain fully saturated 14-membered hexaaza macrocyclic units (1,3,6,8,10,13-hexaazacyclotetradecane) that are linked by $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-N$, $N-(CH_2)_3-N$, or $N-(CH_2)_6-N$ chains. The mononuclear complex $[Cu(H_2L^5)](ClO_4)_4$ ($H_2L^5$ = a protonated form of $L^5$) bearing two $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-NH_2$ pendant arms has also been prepared by the metal-directed reaction of ethylenediamine, 1,2-bis(2-aminoethoxy)ethane, and formaldehyde. The polymer complexes were characterized employing elemental analyses, FT-IR and electronic absorption spectra, molar conductance, X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and scanning electron micrograph (SEM). Electronic absorption spectra of the complexes show that each macrocyclic unit of them has square-planar coordination geometry with a 5-6-5-6 chelate ring sequence. The polymer complexes as well as $[Cu(H_2L^5)]^{4+}$ are quite stable even in concentrated $HClO_4$ solutions. Synthesis and characterization of the polynuclear and mononuclear copper(II) complexes are reported.