• Title/Summary/Keyword: One-pot 합성

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Synthesis of New ${\alpha}$-Amidoketenes Using Malonyl Dihalide (Malonyl Dihalide를 이용한 새로운 ${\alpha}$-Amidoketenes의 합성)

  • Oh, Mi-Jung;Park, Myung-Sook
    • YAKHAK HOEJI
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    • v.55 no.2
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    • pp.127-130
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    • 2011
  • We synthesized new ${\alpha}$-amidoketenes using dehydrochlorination from anilines, triethylamine and malonyl dichloride under $0^{\circ}C$. The utility of ketenes in both laboratory and industrial practice was quickly recognized, and these species have been extensively utilized, including as pharmaceutical intermediates and anti-cancer agents. All synthetic process from anilines to ${\alpha}$-amidoketenes could be carried out by one-pot reaction. Synthetic ketenes 2a~f were identified using NMR and IR spectrum. Formation of ketenes was undertaken with dropping of malonyl dichloride at $0^{\circ}C$ in methylene chloride for 0.5~4 h. Using malonyl dichloride was better than using diethyl malonate as a synthetic reagents for the ketenes.

Nucleophilic Reaction of 2-Phenyl-4-quinolones with Methyl Iodide and Preparation of Its Derivatives (2-Phenyl-4-quinolones와 Methyl Iodide의 친핵반응에 의한 유도체의 합성)

  • Oh, Mi-Jung;Park, Myung-Sook
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.514-519
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    • 2008
  • We developed a convenient synthetic route to 3-alkylated 2-phenyl-4-quinolone derivatives (4a-h and 5a-c), which were expected to retain antitumor activity. A series of 2,3-dihydro-2-hydroxy-2-phenyl-4-quinolones (3a-h) was synthesized through dehydration, dealcoholation and hydration using acid-catalyzed one-pot reaction from anilines and ethyl benzoylacetates. 3-Methyl (or 3,3-dimethyl)-2-phenyl-4-quinolone derivatives 4 and 5 were synthesized from 3a-h through the methylation using methyl iodide. Formation of quinolone nucleus was undertaken with p-toluenesulfonic acid (p-TSA) at $90{\sim}110^{\circ}C$ in toluene for 3${\sim}$7.5 hr over the Dean-Stark apparatus. The key intermediates in these preparations are ${\beta}$-ketoesters 2a-h, which can be readily obtained from the corresponding anilines 1a-e by reaction with ethyl bezoylacetates.

One-pot Synthesis of CdS Nanoparticles by Using $Cd(SOCCH_3)_2Lut_2$ Precusor and Their Optical Characteristics ($Cd(SOCCH_3)_2Lut_2$를 이용한 CdS 나노입자의 용이한 합성 방법 및 광학적 특성)

  • Jang, Seunghyun
    • Journal of Integrative Natural Science
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    • v.2 no.4
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    • pp.285-288
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    • 2009
  • A synthetic route for 12 metal thiocarboxylate complex, $Cd(SOCCH_3)_2Lut_2$ [Lut = 3,5-dimethylpyridine (lutidine)], were investigated for their potential to act as precursors for the formation of cadmium sulfide nanoparticles. $Cd(SOCCH_3)_2Lut_2$ were characterized by 1H-NMR spectroscopy. Thermal decomposition of $Cd(SOCCH_3)_2Lut_2$ is expected to undergo thiocarboxylic anhydride elimination to give stoichiometric cadmium sulfide nanoparticles and removes the organic supporting ligands cleanly. Prepared cadmium sulfide nanoparticles were characterized by fluorescence and UV-vis absorption spectroscopy and displayed an emission band at 500 nm with an excitation wavelength of 360 nm.

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Synthesis of Asymmetric Dimer of Quinolone Derivatives Using p-TSA (p-TSA를 이용한 퀴놀론 유도체의 비대칭 이합체 합성)

  • 박명숙
    • YAKHAK HOEJI
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    • v.48 no.3
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    • pp.202-206
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    • 2004
  • New asymmetric dimers, N,N'-dialkyl-4'-hydroxy-4-oxo-2,2',3,3'-tetrahydro-2,2'-diphenyl-4,4'-quinolones 3a-f were synthesized through the dehydration and dea1coholation of N-alkylanilines and ethyl benzoylacetate. Dimers 3a-f were identified by NMR, IR and GC-MS. A series of dimer 3a-f has been synthesized using acid-catalyzed one-pot reaction that involved the condensation, cyc1ization and dimerization. Similarly, the 6,6'-methoxy (or 7,7'-methoxy) substituted dimers were prepared from N-alkyl-meta-(or para)-anisidines. Formation of dimers was undertaken with p-toluenesulfonic acid (p-TSA) at 90∼11$0^{\circ}C$ in toluene for 2∼6 hours over the Dean-Stark apparatus.

Effects of Arbuscular Mycorrhizal Fungus, Glomus intraradices, on the Growth, Photosynthesis and Phosphorus Content of Robinia pseudoacacia Seedlings Treated with Simulated Acid Rain (Glomus 내생균근균 접종이 인공산성우를 처리한 아까시나무 묘목의 생장, 광합성, 인 함량에 미치는 영향)

  • Kim, Eun Ho;Lee, Kyung Joon;Lee, Kyu Hwa
    • Journal of Korean Society of Forest Science
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    • v.95 no.6
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    • pp.735-742
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    • 2006
  • The objective of this study was to elucidate the tolerance of woody plants to simulated acid rain in relation to mycorrhizal inoculation. Germinating seedlings of Robinia pseudoacacia were planted in 1I pots with autoclaved soil mixture of vermiculite, sand and nursery soil at 1:1:1 ratio. Each pot was inoculated with both crushed root nodules from a wild tree of the same species and commercial arbuscular mycorrhizal inoculum of Glomus intraradices at the time of planting the seedlings. Simulated acid rains at pH 2.6, 3.6, 4.6, and 5.6 were made by mixing sulfuric acid and nitric acid at 3: 1 ratio. Each pot received nutrient solution without N and P, and was also supplied with 180 ml of the one pH level of the acid rains once a week for 50 days. The plants were grown in the green house. At the end of experimental period, plants were harvested to determine contents of chlorophyll, mineral nutrients and net photosynthesis in the tissues, dry weight of the plants, and mycorrhizal infection in the roots. Mycorrhizal infection rate was significantly reduced only at pH 2.6, which meant vitality of G intraradices was inhibited at extremely low pH. Height growth, dry weight production, nodule production and chlorophyll content were increased by mycorrhizal infection in all the pH levels except pH 3.6. Particularly, mycorrhizal inoculation increased root nodule production by 85% in pH 5.6 and 45% in 4.6 treatments. But the stimulatory effect of mycorrhizal inoculation on nodule production was reduced at pH 3.6 and 2.6. Net photosynthesis was increased by mycorrhizal infection in all the pH levels. The phosphorus(P) content in the tissues was increased by 43% in average by mycorrhizal inoculation, which was statistically significant except in pH 2.6. It was concluded that mycorrhizal inoculation of Robinia pseudoacacia would enhance growth and resistance of the plants to acid rain by improving the photosynthesis, phosphorus nutrition, and more nodule production.

Separation of Aluminum and Iron from Platinum Mixture using Synthetic Extraction Resins (합성(合成) 추출(抽出) 수지(樹脂)를 이용(利用)한 백금용액(白金溶液)으로부터 알루미늄과 철(鐵)의 분리(分離))

  • Lim, Gwang-Il;Han, Dong-Hyuk;Hwang, In-Sung;Han, Choon;Lee, Jin-Young;Kim, Joon-Soo;Park, Hyung-Kyu
    • Resources Recycling
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    • v.20 no.3
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    • pp.68-76
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    • 2011
  • For the separation of aluminum and iron from platinum mixtures, extraction resins were synthesized and separation efficiencies were compared with those by commercial one, $P_{204}$. During synthesis, the suspension polymerization method was adopted with D2EHPA as an extractant. Also, benzoyl peroxide as a starter was divided into 3parts and injected for the uniform size and dispersion of resin particles. Comparison tests resulted in 100% separation of Fe and Pt for both synthetic and $P_{204}$ resins. In case of Al and Pt, synthetic and $P_{204}$ resin gave extraction efficiencies of 99.9% and 98.9%, respectively. Difference in extractant contents of synthetic resin(61.8%) and $P_{204}$(60%) was considered to give differences in separation efficiencies of aluminum and iron elements. For both resins, separation efficiencies of Al and Fe increased up to $55^{\circ}C$. According to FT-IR analyses of both resins, specific peaks of D2EHPA and crosslinked polystyrene were identified at the wavenumber of $1000cm^{-1}$ and $2900cm^{-1}$ respectively.

A Study on the Development of Poly-Urea for Porcelain Restoration (폴리우레아 도자기 복원 재료의 적용)

  • Han, Won-Sik;Wi, Koang-Chul;Oh, Seung-Jun;Lee, Young-Hoon
    • Journal of Conservation Science
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    • v.34 no.1
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    • pp.23-29
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    • 2018
  • This study synthesized poly-urea and used it as a filler material for the restoration of porcelain. The synthesized poly-urea was manufactured as a resin and hardener mix that does not undergo contraction during curing, and is unfading. Given an adhesion strength of $180kg/cm^2$ and shearing strength of $200kg/cm^2$, the synthesized poly-urea exhibited the same efficacy as the epoxy putty currently sold in the market. Moreover, it also overcame the drawback of foaming encountered by urethane restoratives, which are a structurally similar type. The hardening time and pot life could also be controlled using additives. The poly-urea used for the restoration of modern artifacts presented a pot life of approximately one hour and took 12 h for complete hardening ($T_{90}$). When a $2{\times}2{\times}2cm$-sized test sample was added to xylene, poly-urea started to separate approximately two hours later and completed perfect pulverization within the solution 24 h later, demonstrating its reversibility. When directly applied to contemporary artifacts, it demonstrated the potential for restoration, as well as convenience and colorfulness.

Synthesis of Naphthacenone Derivatives Using a Michael Reaction (Michael 반응을 이용한 Naphthacenone 유도체의 합성)

  • Rho, Young S.;Yoo, Jin H.;Park, Si H.;Cho, In H.;Kwon, Yoon J.
    • Journal of the Korean Chemical Society
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    • v.40 no.7
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    • pp.519-525
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    • 1996
  • 3-Carbomethoxy-1(3H)-isobenzofuranone(9) underwent condensation with ${\alpha}{\beta}-unsaturated$, esters 3a-b to produce the corresponding naphthacene-6,7-diones 11a-b with high yields in one pot procedure. Among the naphthacene-6,7-diones formed, compound 11a without an ethyl group at C-9 position was oxidized to give the naphthacene-5,12-dione 13a, while compound 11b containing the ethyl group was oxidized to give a 3:2 mixture of the naphthacene-5,7,12-trione 12b and naphthacene-5,12-dione 13b under the same experimental conditions.

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Methane Conversion to Hydrogen Using Ni/Al2O3 Catalyst (Ni/Al2O3 촉매를 이용한 메탄의 수소 전환)

  • Kim, Jun-Keun;Park, Joo-Won;Bae, Jong-Soo;Kim, Jae-Ho;Lee, Jae-Goo;Kim, Younghun;Han, Choon
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.466-470
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    • 2008
  • The objective of this study is to convert methane into hydrogen using a nanoporous catalyst in the $CO_2$ containing syngas generated from the gasified waste. For the purpose, $Ni/Al_2O_3$ catalyst was prepared with the one-pot method. According to analyses of the catalyst, three dimensionally linked sponge shaped particles were created and the prepared nanoporous catalysts had larger surface area and smaller particle size and more uniform pores compared to the sphere shaped commercial catalyst. The catalyst for reforming reaction gave the highest $CH_4$ conversion of 91%, and $CO_2$ conversion of 92% when impregnated with 16 wt% of Ni at the reaction temperature of $750^{\circ}C$. At that time, the prepared catalyst remarkably improved the $CH_4$ and $CO_2$ conversion up to 20% compared to the commercial one.

Carbonylation of Bromobenzyl Bromide Catalyzed by $Co_2(CO)_8(II)$. Selective Synthesis of Alkyl(alkoxymethyl)benzoate (코발트 카르보닐 촉매에 의한 브로모벤질 브로미드의 카르보닐화 (II). 알킬(알콕시메틸)벤조에이트의 선택성 합성)

  • Shim Sang Chul;Doh Chil Hoon;Youn Young Zoo;Cho Chan Sik;Woo Byung Won;Oh Dae Hee
    • Journal of the Korean Chemical Society
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    • v.35 no.1
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    • pp.90-95
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    • 1991
  • A method for the selective syntheses of alkyl (alkoxymethyl)benzoates from halobenzyl halides by two steps in one pot process is described. In the first step, benzyl halide moiety is etherified with alkoxide anion in alcohol by Williamson ether process. In the second step, aryl halide moiety is carbonylated to give alkyl (alkoxymethyl)benzoate with alcohol, Na$_2$CO$_3$, CH$_3$I, and carbon monoxide (1 atm) in the presence of a catalytic amount of Co$_2$(CO)$_8$ in excellent yield.

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