• Title/Summary/Keyword: Solid phase synthesis

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Efficient Macrocyclization for Cyclicpeptide Using Solid-Phase Reaction

  • Kim, Joong-Hup;Hong, Il-Khee;Kim, Hyo-Jeong;Jeong, Hyeh-Jean;Choi, Moon-Jeong;Yoon, Chang-No;Jeong, Jin-Hyun
    • Archives of Pharmacal Research
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    • v.25 no.6
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    • pp.801-806
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    • 2002
  • Cyclicpeptides are important targets in peptide synthesis because of their interesting biological properties. Constraining highly flexible linear peptides by cyclization is one of the mostly widely used approaches to define the bioactive conformation of peptides. Cyclic peptides often have increased receptor affinity and metabolic stability over their linear counterparts. We carried out virtual screening experiment via docking in order to understand the interaction between HLE-Human Leukocyte Elastase and ligand peptide and to identify the sequence that can be a target in various ligand peptides. We made cyclic peptides as a target base on Metlle-Phe sequence having affinity for ligand and receptor active site docking. There are three ways to cyclize certain sequences of amino acids such as Met-lie-Phe-Gly-Ile. First is head-to-tail cyclization method, linking between N-terminal and C-terminal. Second method utilizes amino acid side chain such as thiol functional group in Cys, making a thioether bond. The last one includes an application of resin-substituted amino acids in solid phase reaction. Among the three methods, solid phase reaction showed the greatest yield. Macrocyclization of Fmoc-Met-Ile-Phe-Gly-Ile-OBn after cleavage of Fmoc protection in solution phase was carried out to give macrocyclic compound 5 in about 7% yield. In the contrast with solution phase reaction, solid phase reaction for macrocyclization of Met-Ile-Phe-Gly-Ile-Asp-Tentagel in normal concentrated condition gave macrocyclic compound 7 in more than 35% yield.

Separation of Caffeine and Catechin Compounds from Green Tea by Quercetin Molecular Imprinted Solid-Phase Extraction (케르세틴 분자각인 고정상 추출을 이용한 녹차에서 카페인 및 카테킨 화합물의 분리)

  • Jin, Yin-Zhe;Row, Kyung-Ho
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.165-170
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    • 2007
  • In this work, caffeine and some catechin compounds such as +C, EGC and EGCG were extracted from green tea using quercetin molecular imprinted polymers in solid-phase extraction. For synthesis of MIP, quercetin as the templates, MAA as the monomer, EGDMA as the crosslinker and AIBN as the initiator were used. For extraction of caffeine and catechin compounds from green tea, the solid-phase extractions of a load followed by wash and elution procedures were done with water, methanol and methanol:acetic acid=90:10 (vol.%) as the solvents, respectively. HPLC analysis (C18 column, 5 μm, 250×4.6 mm) with the mobile phase of methanol:water=40:60 (vol.%) at a flow rate of 0.5 ml/min was adopted for the quantitative determination. By solid-phase extraction, the resolutions of caffeine and some catechin compounds from green tea were increased. The quercetin-MIP had higher selectivity to +C compounds.

Synthesis of Solid Electrolyte Nasicon by Solid State Reaction

  • Kim, Cheol-Jin;Chung, Jun-Ki;Lim, Sung-Ki;Rhee, Meung-Ho
    • The Korean Journal of Ceramics
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    • v.2 no.1
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    • pp.25-32
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    • 1996
  • Solid electroyte nasion was synthesized by the optimized solid state reaction minimizing the volume fraction of secondary $ZrO_2$ and glassy phases. To compensate for the evaporation of Na and P during heat-treatment, excess Na and P were added to the starting composition $Na_{1+x} Zr_2 Si_x P_{d-x} O_{12}$ (x=2.1). Phases pure nasicon comparable in volume fraction to the one obtaied from sol-gel process were synthesized after the reaction at $1100~1150^{\circ}C$,$ P_{O2}>=0.1-0.15 $$ZrO_2$ increased with the heat-treatment time due to the decomposition of nasicon phase and that of glassy phase increased as partial oxygen pressure decreased. The synthesized nasion showed a good electrical conductivity of $-1{\times}10^{-2}({\omega}{\cdot}cm)^{-1}$ at $350^{\circ}C$.

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Synthesis of Mullite Whiskers by Vapor-Solid Reaction in the System of Al(OH)3-SiO2-AlF3 (Al(OH)3-SiO2-AlF3계에서 기상-고상반응에 의한 뮬라이트 휘스커 합성)

  • Lee, Hong-Lim;Kang, Jong-Bong
    • Journal of the Korean Ceramic Society
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    • v.43 no.6 s.289
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    • pp.376-382
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    • 2006
  • In the $Al(OH)_3-SiO_2-AlF_3$ system, leaf-shaped fluorotopaz was first formed at $800^{\circ}C$ and mullite whisker was formed at $1,100^{\circ}C$. The mass transportation of Al and Si as gas phase, the fast reaction and growth, and the absence of liquid phase existence in mullite whisker showed that the formation and growth of mullite was from the solid-vapor reaction.

Smart Solid State Syntheses of Well-Crystallized Phase Pure Mixed Oxides for Electroceramics

  • Sennat, Mamoru
    • Journal of the Korean Ceramic Society
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    • v.43 no.11 s.294
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    • pp.680-687
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    • 2006
  • An overview is given to optimize the solid state processes toward phase pure and well-crystallized fine particulates of mixed oxides, serving as electroceramic materials in various genres. Elevation of the reactivity and preservation of stoichiometry of the starting mixture are of universal importance. Mechanical activation is versatile for these purposes, particularly when an oxygen atom as a hinge promotes formation of hetero-bridging bonds between dissimilar cationic species prior to calcination. Case studies carried out recently in the author's laboratory are displayed and compared for ferroelectric materials, i.e. $PbMg_{1/3}Nb_{2/3}O_3$ $xPbTiO_3$(PMN-PT), $(1-y)Pb(Zn_xMg{1-x})_{1/3}$ $yNb_{2/3}O_3$ (PZN-PMN), $BaBi_2Ta_2O_9$ (BBT), $Ba(Mg_{1/3}Ta_{2/3})O_3$ (BMT), and ferromagnetics, i.e. M-, Y-, and Z-phases of Ba-hexaferrites.

Effects of Induction Heating Conditions on Ni-Al Based Intermetallic Compound Coating (Ni-Al계 금속간화합물 코팅에 미치는 고주파유도 가열 조건의 영향)

  • Lee, Han-Young;Kim, Tae-Jun;Cho, Yong-Jae
    • Korean Journal of Metals and Materials
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    • v.48 no.2
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    • pp.141-147
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    • 2010
  • An Ni-Al intermetallic coating has been produced by induction heating on mild steel. The effect of the induction heating conditions on the microstructure of the coating has been investigated. The reaction synthesis of the intermetallic compounds was promoted while increasing the heating rate and the holding time at reaction temperature. Especially, an NiAl phase corresponding to the initial composition of mixed powder was predominantly formed. However, the synthesis at low reaction temperatures occurred by solid state diffusion during the holding time and an Fe-Al reaction layer was formed at the interface with the substrate, regardless of the heating rate. The combustion synthesis of the intermetallic compound occurred at a temperature higher than 1023 K and resulted in an almost single phase NiAl structure.

Chemical Synthesis and Cloning of Panax ginseng Peptide Gene

  • Zhang, Hong-Ying;Chen, Dong-Song;Zhang, Jin
    • Proceedings of the Ginseng society Conference
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    • 1990.06a
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    • pp.65-67
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    • 1990
  • The sequence of ginseng peptide gene was designed and synthesized by the solid phase plasmid pUC19. Escherichia coli JM101 cells were transformed with above hybrid plasmids. Ampicillin resistant transformants were screened and identified by in situ colony hybridization and Southern blot techinques. Finally the gene sequencing was done by the Sanger dideoxy method using primer extension.

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Chemical Synthesis and Cloning of Panax ginseng Peptide Gene (인삼펩티드 유전자의 합성 및 클로닝)

  • Zhang, Hong-Ying;Chen, Dong-Song;Zhang, Jin
    • Journal of Ginseng Research
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    • v.14 no.2
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    • pp.207-209
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    • 1990
  • The sequence of ginseng peptide gene was designed and synthesized by the solid phase phosphoramidiate method. Synthetic segments were isolated, pllrified and joined to the plasmid pUC19. E.icherichiu coli JM101 cells were transformed with above hybrid plasmids. AmpiciIBin resistant transformants were screened and identified by in situ colony hybridization and Southern blot techniques. Finally the gene sequencing was done by the Sanger dideoxy method using primer extension.

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Efficient Solid Phase Library Synthesis of 7 -Alkoxy-1,3,4,5-tetrahydro-benzo [e][ 1.4] diazepin-2-one

  • Im, Isak;Kim, Yong-Chul
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.342.2-342.2
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    • 2002
  • The ${\beta}$-turn has been implicated as an important conformation for biological recognition of peptides or proteins. Benzodiazepine classes have been known as one of the non peptide ${\beta}$-turn mimic scaffolds. We have developed an efficient approach for the synthesis and derivatization of a scaffold of hydroxytetrahydrodizepinone class in order to screen compound library in various protein targets for new lead generations as well as for structure activity relationships of the scaffold. (omitted)

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Hydrothemal Synthesis of $PbTiO_3$ Powders (수열법에 의한 $PbTiO_3$ 분말 합성)

  • 박병규;이태근;이기강
    • Journal of the Korean Ceramic Society
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    • v.33 no.4
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    • pp.399-404
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    • 1996
  • Hydrothemal synthesis of PbTiO3 has been investigated. A comprehensive thermodynamic model for heteroge-nous reacting solid-aquous system has been used to predict the optimum condition for the synthesis. Synthesis were performed using lead acetate trihydrate as Pb source crystalline TiO2 as Ti source and KOH as minerali-zer. The synthesis has been examined at low temperature (16$0^{\circ}C$) Phase pure perovskite PbTiO3 has been obtained at high pH(above 0.5 mol KOH). The morphology of PbTiO3 was acicular shape. It has been found sible for a distortion in the c direction. The water is gradully released on annealing the powder to 40$0^{\circ}C$ and the normal crystallographic properties are restored.

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