• Title/Summary/Keyword: 용매화 수

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A Newer Short Synthesis of dl-Muscone(Ⅰ) (새로운 짧은 경로로의 dl-Muscone 합성(Ⅰ))

  • Im, D.S.;Shin, D.H.;Park, D.K.
    • Journal of the Korean Chemical Society
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    • v.40 no.4
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    • pp.243-248
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    • 1996
  • New routes have been developed for the practical syntheses of dl-Muscone(1) employing cyclopentadecanone(2) as the starting material. In this experiment, addition of bromine to cyclopentadecanone in dried E. Ether solution with a trace of $AlCl_3$ as the catalyst were produced 2-bromocyclopentadecanone(3). This process was enhanced formation of regioselective enolate anion at $C_2$ position. 2-Bromocyclopentadecanone was put into $Li_2CO_3$-LiBr-DMF solution at 140∼150$^{\circ}C$, were produced trans- and cis-2-cyclopentadecen-1-one(4) mixture. Other by-products were reduced by control of reaction temperature and time. Trans- and cis-2-cyclopentadecen-1-one(4) mixture was directly put into dried E. Ether solvent and induce to react dropwise with $CH_3MgBr-Cu_2Cl_2$ complex, all of them got into 1,4-addition, dl-Muscone (1) was formed as the result. Conculsion, through three steps procedure from cyclopentadecanone(2) to dl-Muscone(1), the pure dl-Muscone was obtained with the high proportion of 85%, and synthetic cost was able to be much lower than any other conventional methods as there were no chemical separating steps.

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Extraction Characteristics of Saponin and Acidic Polysaccharide Based on the Red Ginseng Particle Size (홍삼의 입자크기에 따른 사포닌 및 산성다당체의 추출 특성)

  • Cho, Chang-Won;Kim, Sang-Wook;Rho, Jeong-Hae;Rhee, Young-Kyung;Kim, Kyung-Tack
    • Journal of Ginseng Research
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    • v.32 no.3
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    • pp.179-186
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    • 2008
  • Effect of pulverization on total solid, crude saponin, and acidic polysaccharide contents of dried red ginseng main root were tested. Several particle size samples, including red ginseng main root (non pulverized), $10{\sim}40$ mesh powder, $40{\sim}100$ mesh powder, and >100 mesh powder were used in the extraction. The sequential solvent extraction method (1st: 70% EtOH at $70^{\circ}C$ for 12 hr, 2nd: 70% EtOH at $70^{\circ}C$ for 12 hr, 3rd: water at $70^{\circ}C$ for 12 hr) was applied to extract the saponins and acidic polysaccharide. Extraction yield of total solid of pulverized red ginseng ($10{\sim}40$ mesh size) was increased to 20% compared with that of non-pulverized. Especially, the crude saponin content of pulverized red ginseng ($10{\sim}40$ mesh size) showed an increase of 47% over non-pulverized. No difference in the component ratio was observed by pulverization, when the individual ginsenosides were quantified by HPLC. Also, extraction yield of acidic polysaccharide of pulverized red ginseng ($10{\sim}40$ mesh size) was increased 57% compared with that of non-pulverized. The results suggested that pulverization might be useful for increasing the extraction yield of red ginseng components.

Study of Polysulfone Membrane for Membrane-covered Oxygen Probe System (산소 전극 시스템에 사용되는 polysulfone막에 대한 연구)

  • Hong, Suk In;Kim, Hyun Joon;Park, Hee Young;Kim, Tae Jin;Jeong, Yong Seob
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.877-887
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    • 1996
  • The ideal membranes for membrane-covered oxygen probes system should be selectively permeable for oxygen and chemically inert, and have good mechanical strength. Polysulfone(PSf) was selected to develop the membrane for membrane-covered oxygen electrodes system. PSf membranes have properties such as good reproducibility, good mechanical strength, chemical inertness, and high heat resistance. PSf membranes were cast from polymer solution on the glass plate at constant temperature, and casting solvents used were tetrahydrofuran(THF), methylene chloride, and N-methyl-2-pyrrolidone(NMP). Tricresyl phosphate(TCP) as plasicizer was added to PSf to increase the softness of membrane. The permeation characteristics were observed for pure oxygen and nitrogen through pure PSf membranes by variable volume method and membrane-covered electrode system. The permeability coefficients of oxygen and nitrogen measured by variable volume method were slightly decreased with increasing of upstream pressure. The permeation properties of PSf membrane using methylene choride as casting solvent were not affected by the PSf amount of polymer solution. The permeability coefficients of oxygen and nitrogen for PSf membrane containing TCP were very slightly lower than those for pure PSf membrane, but ideal separation factors were slightly higher. The flexibility of PSf membrane containing 2wt% TCP was better than that of pure PSf membrane. It was expected that this increase in flexibility would solve the difficulty of fixing the membrane to the cathode. The membrane-covered oxygen probes system was composed of anode, cathode and electrolyte. The type of the anode was Ag/AgCl half-cell, that of cathode was Ag, and the electrolyte was 4N KCl solution. The result of sampled current voltametry for PSf membrane showed the plateu region at -0.3V~-1.0V. The correlation coefficient of oxygen partial pressure versus current for PSf membrane was relatively high, 0.99949. It was concluded that PSf membrane was the good candidate for the membrane-covered oxygen probes system.

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Anti-wrinkle Activity of $\beta$-carotene Extracted & Purified from Recombinant Escherichia coli (재조합 대장균으로부터 추출.정제된 베타-카로틴의 주름개선 활성)

  • Jo, Ji-Song;Ku, Bo-Mi;Kang, Sang-Soo;Lee, Jae-Ran;Kim, You-Geun;Lee, He;Kim, Sung-Bae;Kim, Seon-Won;Kim, Chang-Joon;Chung, In-Young
    • KSBB Journal
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    • v.23 no.6
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    • pp.513-518
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    • 2008
  • This paper described the extraction/purification of $\beta$-carotene from recombinant E.coli and evaluation of anti-wrinkle activity of purified $\beta$-carotene. No significant differences in extraction yields were observed when hexane or isobutyl acetate was used. However, extraction from wet-cell cake resulted in 2-fold higher amount of $\beta$-carotene than that from dry cells. Disruption of 5 g-wet cells by ultrasonic homogenizer, acetone dehydration, extraction with isobutyl acetate resulted in 36 mg of $\beta$-carotene corresponding to 61.2% of recovery. The formation and separation of $\beta$-carotene crystal improved the purity. 633 mg of $\beta$-carotene crystal with 93% purity was obtained from 223 g/L of wet-cell cake harvested from 2.5-L fed-batch culture broth. The cultures of normal human primary fibroblast were performed to investigate the effect of $\beta$-carotene on cytotoxicity as MTT assay and anti-wrinkle activity as collagen synthesis assays. $1.7{\mu}M$ of $\beta$-carotene was found to be optimal concentration at which 1.4-fold higher amount of collagen was synthesized than that in absence of $\beta$-carotene. This indicates that highly purified $\beta$-carotene can be obtained from recombinant E.coli by applying simple method with less toxic solvent and can be used in functional cosmetics as anti-wrinkle agent.

Solvothermal Preparation of Nanocrystalline TiO2 Using Alcohol-water Mixed Solvent (알코올-물 혼합용액을 이용하는 Solvothermal 법에 의한 나노크기의 TiO2 제조)

  • Lee, Sang Geun;Park, Seong Soo;Hong, Seong Soo;Park, Jong Myung;Lee, Seung Ho;Kim, Dae Sung;Lee, Gun Dae
    • Applied Chemistry for Engineering
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    • v.22 no.6
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    • pp.685-690
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    • 2011
  • In this study, a solvothermal reaction to prepare nanocrystalline titania was carried out using $TiCl_4$ and mixed solvents of alcohol and water. The effects of the type and the composition of alcohol on the crystal structure and agglomeration of final $TiO_2$ products were investigated. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscopy (SEM). In the solvothermal reaction using the n-butanol solutions with different volume ratios of n-butanol/water (100/0, 75/25, 50/50, 25/75, 0/100), the extent of agglomeration of obtained rutile $TiO_2$ was found to change with the volume ratio of n-butanol/water, and the n-butanol/water ratio of 75/25 revealed the best result for the preparation of well-dispersed nanocrystalline $TiO_2$ powders. The crystal phase of $TiO_2$ prepared through the solvothermal reaction changed with the type of alcohol in solvent (alcohol/water = 75/25). $TiO_2$ products obtained with the aqueous solutions of methanol, ethanol and isopropanol have an anatase phase, while that with n-butanol has a rutile phase. The results showed that, in the solvothermal reaction using both $TiCl_4$ as a starting material and the alcohol-water mixed solvents without any other additive, the enhancement of dispersion and control of crystal structure of $TiO_2$ products can be feasible by simply varying the composition and type of alcohol in the mixed solvents.

Silica/polymer Nanocomposite Containing High Silica Nanoparticle Content : Change in Proton Conduction and Water Swelling with Surface Property of Silica Nanoparticles (고농도의 Silica Nanoparticle을 함유한 Silica/polymer 나노복합체 : 실리카 표면 특성에 따른 수소이온 전도성 및 수팽윤도 변화)

  • Kim, Ju-Young;Kim, Seung-Jin;Na, Jae-Sik
    • Applied Chemistry for Engineering
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    • v.21 no.5
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    • pp.514-521
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    • 2010
  • A new one-shot process was employed to fabricate proton exchange membranes (PEMs) over conventional solvent-casting process. Here, PEMs containing nano-dispersed silica nanoparticles were fabricated using one-shot process similar to the bulk-molding compounds (BMC). Different components such as reactive dispersant, urethane acrylate nonionmer (UAN), styrene, styrene sulfuric acid and silica nano particles were dissolved in a single solvent dimethyl sulfoxide (DMSO) followed by copolymerization within a mold in the presence of radical initiator. We have successfully studied the water-swelling and proton conductivity of obtained nanocomposite membranes which are strongly depended on the surface property of dispersed silica nano particles. In case of dispersion of hydrophilic silica nanoparticles, the nanocomposite membranes exhibited an increase in water-swelling and a decrease in methanol permeability with almost unchanged proton conductivity compared to neat polymeric membrane. The reverse observations were achieved for hydrophobic silica nanoparticles. Hence, hydrophilic and hydrophobic silica nanoparticles were effectively dispersed in hydrophilic and hydrophobic medium respectively. Hydrophobic silica nanoparticles dispersed in hydrophobic domains of PEMs largely suppressed swelling of hydrophilic domains by absorbing water without interrupting proton conduction occurred in hydrophilic membrane. Consequently, proton conductivity and water-swelling could be freely controlled by simply dispersing silica nanopartilces within the membrane.

Electrochemical Study on Transfer Reaction of Ionizable Cefotiam across a Water/1,2-dichloroethane Interface and Drug Sensing Applications (물/1,2-Dichloroethane 계면에서 Cefotiam 약물 이온의 전이 반응 연구 및 약물 센서에 응용)

  • Liu, XiaoYun;Jeshycka, Shinta;Lee, Hye Jin
    • Applied Chemistry for Engineering
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    • v.29 no.5
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    • pp.581-588
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    • 2018
  • In this article, electrochemical investigation of the transfer reaction of ionizable cefotiam (CTM), an antibiotic molecule across a polarized water/1,2-dichloroethane (water/1,2-DCE) interface was studied. Ion partition diagram providing the preferred charged form of CTM in either water or 1,2-DCE phase was established via the voltammetric evaluation of the transfer process of differently charged CTM species depending upon the pH variation of aqueous solutions. Thermodynamic information including the formal transfer potential and formal Gibbs transfer energy values in addition to important pharmacokinetics including partition coefficients of ionizable CTM were also evaluated. In particular, the current associated with the transfer of CTM present at pH 3.0 aqueous solution proportionally increased with respect to the CTM concentration which was further used for developing CTM sensitive ion sensor. In order to improve the portability and convenient usage, a single microhole interface fabricated in a supportive polyethylene terephthalate film was used of which hole was filled with a polyvinylchloride-2-nitrophenyloctylether (PVC-NPOE) gel replacing 1,2-DCE, a toxic organic solvent. A dynamic range of $1-10{\mu}M$ CTM was obtained.

Biosensor System for the Detection of Agrichemicals and Its Applications (농약 검출을 위한 바이오센서 시스템 연구 및 그 응용)

  • Park, Tae-Jung;Yang, Min-Ho;Lee, Sang-Yup;Kim, Soo-Hyun
    • KSBB Journal
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    • v.24 no.3
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    • pp.227-238
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    • 2009
  • In the recent years, some organic toxic chemicals were used for obtaining high-yield productivity in agriculture. The undegraded pesticides may remain in the agricultural foods through atmosphere, water, and soil and cause public health problems to environmental resources and human beings even at very low concentrations. Small amounts of pesticides can affect a central nervous system, resulting in immunogenic diseases, infertility problems, respiratory diseases and born marrow diseases, which can lead even to death. Monitoring of the environmental pesticide is one of the important issues for the human well-being. Several kinds of biosensors have been successfully applied to the detection of agrichemical toxicity. Also, few platforms for biocide detection have been definitely developed for the degradation and reaction of pesticides. Biochip and electrochemistry experiments involve immobilizing a receptor molecule on a solid substrate surface, and monitoring its interaction with an analyze in a sample solution. Furthermore, nanotechnology can be applied to make high-throughput analyses that are smaller, faster and sensitive than conventional assays. Some nanomaterials or nanofabricated surfaces can be coupled to biomolecules and used in antibody-based assays and enzymatic methods for pesticide residues. The operation procedure has become more convenient as it does not require labeling procedure. In this paper, we review the recent advances in agrichemical defection research and also describe the label-free biosensor for pesticides using various useful detection methods.

Synthesis of a Perfluoropolyether Intermediate via Electrophilic Fluorine-Substituting Direct Fluorination (친전자성 불소치환 직접플루오르화 반응에 의한 Perfluoropolyether 중간체의 합성)

  • Yun, Seok-Min;Lim, Jae-Won;Jeong, Eui-Gyung;Park, In-Jun;Lee, Young-Seak
    • Polymer(Korea)
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    • v.35 no.2
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    • pp.166-170
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    • 2011
  • This study reported the synthesis of perfluoropolyether intermediate (TP-$COOCF_3$) having a $CF_3$ functional group via electrophilic fluorine substituting direct fluorination from PFPE intermediate (TP-$COOCH_3$) having a $CH_3$ functional group, which was synthesized by the ring opening polymerization and methyl esterification of HFPO. The effects of reaction conditions such as the amount of solvent, fluorine partial pressure, reaction time, were investigated. The results showed that the yield of fluorination reaction became the highest when the reaction was carried out in a mild condition for a long reaction time, which also minimized side reactions. The sample was characterized by FTIR and NMR, which confirmed the synthesis of the final product, TP-$COOCF_3$, via direct fluorination converting $CH_3$ of TP-$COOCH_3$ to $CF_3$ of TP-$COOCF_3$ with 95.4% yield.

Antioxidation Behavior of Submicron-sized Cu Particles with Ag Coating (서브 마이크론급 구리 입자의 은도금 공정에 따른 내산화성 강화 연구)

  • Choi, Eun Byeol;Lee, Jong-Hyun
    • Journal of the Microelectronics and Packaging Society
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    • v.23 no.3
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    • pp.51-56
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    • 2016
  • To fabricate a copper (Cu)-based fine conductive filler having antioxidation property, submicron silver (Ag)-coated Cu particles were fabricated and their antioxidation property was evaluated. After synthesizing the Cu particles of $0.705{\mu}m$ in average diameter by a wet-reduction process, Ag-coated Cu particles were fabricated by successive Ag plating using ethylene grycol solvent. Main process parameters in the Ag plating were the concentration of reductant (ascorbic acid), the injection rate of Ag precursor solution, and the stirring rate in mixed solution. Thus, Ag plating characteristics and the formation of separate fine pure Ag phase were observed with different combinations of process parameters. As a result, formation of the separate pure Ag phase and aggregation between Ag-coated Cu particles could be suppressed by optimization of the process parameters. The Ag-coated Cu particles which were fabricated using optimal conditions showed slight aggregation, but excellent antioxidation property. For example, the particles indicated the weight gain not exceeding 0.1% until $225^{\circ}C$ when they were heated in air at the rate of $10^{\circ}C/min$ and no weight gain until 75 min when they were heated in air at $150^{\circ}C$.