• Title/Summary/Keyword: One-pot synthesis

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Enzymatic Manufacture of Deoxythymidine-5'-Triphosphate with Permeable Intact Cells of E. coli Coexpressing Thymidylate Kinase and Acetate Kinase

  • Zhang, Jiao;Qian, Yahui;Ding, Qingbao;Ou, Ling
    • Journal of Microbiology and Biotechnology
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    • v.25 no.12
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    • pp.2034-2042
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    • 2015
  • A one-pot process of enzymatic synthesis of deoxythymidine-5'-triphosphate (5'-dTTP) employing whole cells of recombinant Escherichia coli coexpressing thymidylate kinase (TMKase) and acetate kinase (ACKase) was developed. Genes tmk and ack from E. coli were cloned and inserted into pET28a(+), and then transduced into E. coli BL21 (DE3) to form recombinant strain pTA in which TMKase and ACKase were simultaneously overexpressed. It was found that the relative residual specific activities of TMKase and ACKase, in pTA pretreated with 20 mM ethylene diamine tetraacetic acid (EDTA) at 25℃ for 30 min, were 94% and 96%, respectively. The yield of 5'-dTTP reached above 94% from 5 mM deoxythymidine 5'-monophosphate (5'-dTMP) and 15 mM acetyl phosphate catalyzed with intact cells of pTA pretreated with EDTA. The process was so effective that only 0.125 mM adenosine-5'-triphosphate was sufficient to deliver the phosphate group from acetyl phosphate to dTMP and dTDP.

Synthesis of a Precursor of Bulgecinine, (4S,5R)-1-Acetyl-2-formyl-5-benzyloxymethyl-4-pyrrolidinol (Bulgecinine 선구물질인 (4S,5R)-1-Acetyl-2-formyl-5-benzyloxymethyl-4-pyrrolidinol의 합성)

  • Jeon, Hak Rim;Yoon, Shin Sook;Shin, Young Sook;Nam Shin, Jeong E.
    • Journal of the Korean Chemical Society
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    • v.41 no.3
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    • pp.150-156
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    • 1997
  • A precursor of bulgecinine, (4S,5R)-1-acetyl-2-formyl-5-benzyloxymethyl-4-pyrrolidinol (15) has been synthesized from diacetone-D-glucose. Barton deoxygenation, conversion to an L-sugar and displacement with $N_3^-$ at C-5, and one-pot reductive cyclization at C-2 produced (6R)-6-Ο-benzyloxymethyl-(3R)-3-methoxy-2-oxa-5-azabicyclo-[2,2,1]heptane(13), a key intermediate for bulgecinine. N-Acetylation and acid hydrolysis of 13 furnished a precursor of bulgecinine, (2S,4S,5R)-pyrrolidinol derivative 15 and its (2R,4S,5R)-diastereomer.

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Green Synthesis of Ag Thin Films on Glass Substrates and Their Application in Surface-Enhanced Raman Scattering

  • Cho, Young Kwan;Kim, In Hyun;Shin, Kuan Soo
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2942-2946
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    • 2013
  • Nanostructured Ag thin films could be facilely prepared by soaking glass substrates in ethanolic solutions containing $Ag_2O$ powders at an elevated temperature. The formation of zero-valent Ag was corroborated using X-ray diffraction and X-ray photoelectron spectroscopy. The deposition of Ag onto a glass substrate was readily controlled simply by changing the reaction time. Due to the aggregated structures of Ag, the surface-enhanced Raman scattering spectra of benzenethiol could be clearly identified using the Ag-coated glass. The enhancement factor at 514.5 nm excitation estimated using benzenethiol reached $1.0{\times}10^5$ while the detection limit of rhodamine 6G was found to be as low as $1.0{\times}10^{-13}$ M. Since this one-pot fabrication method is eco-friendly and is suitable for the mass production of diverse Ag films, it is expected to play a significant role in the development of surface plasmon-based analytical devices.

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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The Synthesis of CuInS2 Nanoparticles by a Simple Sonochemical Method

  • Park, Jae-Young;Park, Jong-Pil;Hwang, Cha-Hwan;Kim, Ji-Eon;Choi, Myoung-Ho;Ok, Kang-Min;Kwak, Ho-Young;Shim, Il-Wun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2713-2716
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    • 2009
  • $CuInS_{2}$ nanoparticles were synthesized by a simple sonochemical method; First, Cu nanoparticles were prepared from $CuInS_{2}$ in methanol solution by a one pot reaction through the sonochemistry under multibubble sonoluminescence (MBSL) conditions. Second, the resulting Cu nanoparticles were treated with $InCl_3{\cdot}4H_2O$ and $CH_3CSNH_2$ (thioacetamide) at the same MBSL conditions to synthesize $In_2S_3$-coated Cu nanoparticles in methanol solution. Then, they were transformed into $CuInS_{2}$ (CIS) nanoparticles of 20 $\sim$ 40 nm size in diameter by thermal heating at 300 ${^{\circ}C}$ for 2 hr. The prepared CIS nanoparticles, of which band gap is 1.44 eV, were investigated by X-ray diffractometer, UV-Vis spectrophotometer, inductively coupled plasma spectrometer, and high resolution-transmission electron microscope.

Synthesis and Characterization of Zn(1-x)NixAl2O4 Spinels as a New Heterogeneous Catalyst of Biginelli's Reaction

  • Akika, Fatima-Zohra;Kihal, Nadjib;Habila, Tahir;Avramova, Ivalina;Suzer, Sefik;Pirotte, Bernard;Khelili, Smail
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1445-1453
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    • 2013
  • $Zn_{(1-x)}Ni_xAl_2O_4$ (x = 0.0-1.0) spinels were prepared at $800^{\circ}C$ by co-precipitation method and characterized by infrared spectroscopy, X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The specific surface area was determined by BET. SEM image showed nano sized spherical particles. XPS confirmed the valence states of the metals, showing moderate Lewis character for the surface of materials. The powders were successfully used as new heterogeneous catalysts of Biginelli's reaction, a one-pot three-component reaction, leading to some dihydropyrimidinones (DHPMs). These new catalysts that produced good yields of DHPMs, were easily recovered by simple filtration and subsequently reused with persistent activity, and they are non-toxic and environmentally friendly. The optimum amount of catalyst is 20% by weight of benzaldehyde derivatives, while the doping amount has been found optimal for x = 0.1.

Synthesis and physicochemical characterization of NixZnx-Fe2O4/MWCNT nanostructures as enzyme mimetics with peroxidase-like catalytic activity

  • Salarizadeh, Navvabeh;Sadri, Minoo;Hosseini, Hassan;Sajedi, Reza. H.
    • Carbon letters
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    • v.24
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    • pp.103-110
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    • 2017
  • Carbon-based magnetic nanostructures in several instances have resulted in improved physicochemical and catalytic properties when compared to multi-wall carbon nanotubes (MWCNTs) and magnetic nanoparticles. In this study, magnetic MWCNTs with a structure of $Ni_xZn_xFe_2O_4/MWCNT$ as peroxidase mimics were fabricated by the one-pot hydrothermal method. The structure, composition and morphology of the nanocomposites were characterized with X-ray diffraction (XRD), Fourier transform infrared spectroscopy and transmission electron microscopy. The magnetic properties were investigated with a vibrating sample magnetometer. The peroxidase-like catalytic activity of the nanocomposites was investigated by colorimetric and electrochemical tests with 3,3',5,5'-tetramethylbenzidine (TMB) and $H_2O_2$ as the substrates. The results show that the synthesis of the nanocomposites was successfully performed. XRD analysis confirmed the crystalline structures of the $Ni_xZn_xFe_2O_4/MWCNT$ nanohybrids and MWCNTs. The main peaks of the $Ni_xZn_xFe_2O_4/MWCNT$s crystals were presented. The $Ni_{0.25}Zn_{0.25}Fe_2O_4/MWCNT$ and $Ni_{0.5}Zn_{0.5}Fe_2O_4/MWCNT$ nanocatalysts showed nearly similar physicochemical properties, but the $Ni_{0.5}Zn_{0.5}Fe_2O_4/MWCNT$ nanocatalyst was more appropriate than the $Ni_{0.25}Zn_{0.25}Fe_2O_4/MWCNT$ nanocatalyst in terms of the magnetic properties and catalytic activity. The optimum peroxidase-like activity of the nanocatalysts was obtained at pH 3.0. The $Ni_{0.5}Zn_{0.5}Fe_2O_4/MWCNT$ nanocatalyst exhibited a good peroxidase-like activity. These magnetic nanocatalysts can be suitable candidates for future enzyme-based applications such as the detection of glucose and $H_2O_2$.

An Efficient Method for Synthesis of PEO-Based Macromonomer and Macroinitiator

  • Kim, Jung-Ahn;Choi, Song-Yee;Kim, Kyung-Min;Go, Da-Hyeon;Jeon, Hee-Jeong;Lee, Jae-Yeol;Park, Hyeong-Soo;Lee, Cheol-Han;Park, Heung-Mok
    • Macromolecular Research
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    • v.15 no.4
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    • pp.337-342
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    • 2007
  • The n-butyllithium-initiated ring-opening polymerization of ethylene oxide, in a mixture of benzene and dimethylsulfoxide (DMSO), between $25-45^{\circ}C$, with potassium tert-butoxide, is a useful and powerful method to control the molecular weight as well as achieve a quantitative chain-end functionalization yield of the resulting polymeric alkoxide via a one pot synthesis. The molecular weight of the product could be controlled by adjusting the ratio of grams of monomer to moles of initiators, such as n-butyllithium ([n-BuLi]) and potassium t-butoxide ([t-BuOK]). The yields for the macromonomer and ${\omega}-brominated$ poly(ethylene oxide) (PEO) were quantitative in relation to the chain-end functionalizations of the polymeric alkoxide formed. The resulting products were characterized by a combination of $^1H-NMR$ spectroscopic and size exclusion chromatographic analyses.

Preparation of Fabric Softener Product by using Amine-functionalized Magnesium-phyllosilicates (아민기로 관능화된 마그네슘-층상규산염을 이용한 섬유유연제 제조)

  • Kim, Seong Yeol;Choi, Yoo-Sung
    • Applied Chemistry for Engineering
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    • v.30 no.5
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    • pp.580-585
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    • 2019
  • In this study, we synthesized amine-functionalized magnesium-phyllosilicates (AF-MgP) with an octahedral and tetrahedral structure using (3-aminopropyl)triethoxysilane. The synthesis of AF-MgP, surface functionalization of amine and 1 : 2 ratio of the octahedral and tetrahedral structure were confirmed by FT-IR and XRD analysis. In addition, it was confirmed that AF-MgP was absorbed evenly on the surface of cotton fibers and coated on the cotton fibers from HR-SEM and EDX analysis. The antimicrobial activity test of cotton fibers according to KS confirmed that cotton fibers coated with AF-MgP particles show an enhanced antimicrobial activity against cutaneous microorganisms. Our results suggest that AF-MgP is not only applied as a functional nanomaterial that gives the cotton fiber antimicrobiality, but also can be used in the field of cosmetic and biomedical materials.

Metal-organic frameworks-driven ZnO-functionalized carbon nanotube fiber for NO2 sensor

  • Woo, Sungyoon;Jo, Mingyeong;Lee, Joon-Seok;Choi, Seung-Ho;Lee, Sungju;Jeong, Hyeon Su;Choi, Seon-Jin
    • Journal of Sensor Science and Technology
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    • v.30 no.6
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    • pp.369-375
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    • 2021
  • In this study, heterogeneous ZnO/CNTF composites were developed to improve the NO2-sensing response, facilitated by the self-heating property. Highly conductive and mechanically stable CNTFs were prepared by a wet-spinning process assisted by the liquid crystal (LC) behavior of CNTs. Metal-organic frameworks (MOFs) of ZIF-8 were precipitated on the surface of the CNTF (ZIF-8/CNTF) via one-pot synthesis in solution. The subsequent calcination process resulted in the formation of the ZnO/CNTF composites. The calcination temperatures were controlled at 400, 500, and 600 ℃ in an N2 atmosphere to confirm the evolution of the microstructures and NO2-sensing properties. Gas sensor characterization was performed at 100 ℃ by applying a DC voltage to induce Joule heating through the CNTF. The results revealed that the ZnO/CNTF composite after calcination at 500 ℃ (ZnO/CNTF-500) exhibited an improved response (Rair/Rgas = 1.086) toward 20 ppm NO2 as compared to the pristine CNTF (Rair/Rgas = 1.063). Selective NO2-sensing properties were demonstrated with negligible responses toward interfering gas species such as H2S, NH3, CO, and toluene. Our approach for the synthesis of MOF-driven ZnO/CNTF composites can provide a new strategy for the fabrication of wearable gas sensors integrated with textile materials.