• 제목/요약/키워드: One-pot synthesis

검색결과 222건 처리시간 0.019초

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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    • 제34권5호
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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.

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

  • 정승호;이재섭;조중상
    • 청정기술
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    • 제30권3호
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    • pp.220-227
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    • 2024
  • 고용량 및 고에너지 밀도의 리튬 이온 전지 수요가 증가함에 따라 기존 흑연 음극을 대체할 고용량 실리콘 음극이 주목받고 있다. 하지만, 실리콘은 충·방전 동안 ~360%의 큰 부피 팽창 및 낮은 이온 전도도와 전기 전도도로 인해 저조한 수명 및 율속 특성을 나타낸다. 해당 문제를 해결하기 위해, 본 연구에서는 Pluronic-F127을 활용한 단일 분무 열분해 공정을 통해 코어@쉘 구조의 실리콘@탄소 나노 분말(Si@C NPs)을 합성한다. 분무 용액 내 Pluronic-F127은 실리콘 나노 입자/dextrin 응집체 형성 억제와 동시에 열분해됨으로써 나노 분말 합성에 기여한다. 또한 dextrin으로부터 유래된 비정질 탄소는 실리콘 입자 표면에 코팅되어 소재 내 전자 이동 경로 역할과 실리콘 나노 입자간 전기적 접촉을 강화한다. 그 결과, Si@C NPs는 1.0 A g-1에서 50 사이클 후 1,912 mA h g-1의 방전 용량 및 높은 율속 특성(3.0 A g-1에서 방전 용량 1,493 mA h g-1)을 나타내었다. 따라서 본 연구에서 제시한 분무 열분해 공정 기반 실리콘@탄소 복합 나노 분말 합성 전략은 실리콘 음극 소재 성능 향상에 새로운 방향을 제시할 수 있을 것으로 기대한다.

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

  • 박홍수;홍석영;김송형;유규열;안성환;함현식
    • 한국응용과학기술학회지
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    • 제23권4호
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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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    • 제31권8호
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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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    • 제35권6호
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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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    • 제31권8호
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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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    • 제32권7호
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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.

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

  • 이재욱;한승철;김희주;김정환;이언엽;김병기;성새름;강화신;김지현;허도성
    • 폴리머
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    • 제31권5호
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    • pp.417-421
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    • 2007
  • 덴드리틱 벤질 알코올을 트리에틸아민과 메탄술포닐클로라이드와 반응시켜서, 덴드리틱 벤질 클로라이드의 효율적인 합성이 이루어졌다. 이 반응은 히드록시기의 메실화 반응과 염소화 반응의 2단계 반응으로 이루어지는데, 중간체의 분리없이 한 반응 용기내에서 반응이 진행되는 경제적인 방법이다.

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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    • 제1권1호
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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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    • 제33권8호
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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.