• Title/Summary/Keyword: Syntheses

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Syntheses and Characterizations of Serine and Threonine Capped Water-Dispersible ZnS:Mn Nanocrystals and Comparison Study of Toxicity Effects on the growth of E. coli by the Methionine, Serine, Threonine, and Valine Capped ZnS:Mn Nanocrystals

  • Lim, Eun-Ju;Park, Sang-Hyun;Byun, Jong-Hoe;Hwang, Cheong-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1741-1747
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    • 2012
  • Water-dispersible ZnS:Mn nanocrystals were synthesized by capping the surface of the nanocrystals with conventional aminoacids ligands: serine and threonine. The aminoacids capped ZnS:Mn nanocrystal powders were characterized by XRD, HR-TEM, EDXS, ICP-AES and FT-IR spectroscopy. The optical properties were also measured by UV/Vis and solution photoluminescence (PL) spectroscopies in aqueous solvents. The solution PL spectra showed broad emission peaks around 600 nm with PL efficiencies of 9.7% (ZnS:Mn-Ser) and 15.4% (ZnS:Mn-Thr) respectively. The measured particle sizes for the aminoacid capped ZnS:Mn nanocrystals by HR-TEM images were about 3.0-4.0 nm, which were also supported by Debye-Scherrer calculations. In addition, cytotoxic effects of four aminoacids capped ZnS:Mn nanocrsystals over the growth of wild type E. coli were investigated. Although toxicity in the form of growth inhibition was observed with all the aminoacids capped ZnS:Mn nanocrystals at higher dose (1 mg/mL), ZnS:Mn-Met and ZnS:Mn-Thr appeared non-toxic at doses less than 100 ${\mu}g$/mL. Low biological toxicities were seen at doses less than 10 ${\mu}g$/ mL for all nanocrystals.

Enhancement in the Photocatalytic Activity of Au@TiO2 Nanocomposites by Pretreatment of TiO2 with UV Light

  • Khan, Mohammad Mansoob;Kalathil, Shafeer;Lee, Jin-Tae;Cho, Moo-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1753-1758
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    • 2012
  • A novel, efficient and controlled protocol for the synthesis and enhanced photocatalytic activity of $Au@TiO_2$ nanocomposite is developed. $TiO_2$ (P25) was pretreated by employing UV light (${\lambda}$ = 254 nm) and the pretreated $TiO_2$ was uniformly decorated by gold nanoparticles (AuNPs) in presence of sodium citrate and UV light. UV pretreatment makes the $TiO_2$ activated, as electrons were accumulated within the $TiO_2$ in the conduction band. These accumulated electrons facilitate the formation of AuNPs which were of very small size (2-5 nm), similar morphology and uniformly deposited at $TiO_2$ surface. It leads to formation of stable and crystalline $Au@TiO_2$ nanocomposites. The rapidity (13 hours), monodispersity, smaller nanocomposites and easy separation make this protocol highly significant in the area of nanocomposites syntheses. As-synthesized nanocomposites were characterized by TEM, HRTEM, TEM-EDX, SAED, XRD, UV-visible spectrophotometer and zeta potential. Dye degradation experiments of methyl orange show that type I ($Au@TiO_2$ nanocomposites in which $TiO_2$ was pretreated with UV light) has enhanced photocatalytic activity in comparison to type II ($Au@TiO_2$ nanocomposites in which $TiO_2$ was not pretreated with UV light) and $TiO_2$ (P25). This shows that pretreatment of $TiO_2$ provides type I a better catalytic activity.

Exploration and functional expression of homologous lipases of Candida antarctica lipase B (Candida antarctica lipase B의 상동체 효소 탐색과 발현)

  • Park, Seongsoon
    • Korean Journal of Microbiology
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    • v.51 no.3
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    • pp.187-193
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    • 2015
  • Candida (also known as Pseudozyma) antarctica lipase B (CAL-B) has been intensely studied in academic and industrial fields. However, the research related to its homologous enzymes has been rarely reported. In the current investigation, protein sequence similarity search of CAL-B has been conducted and six homologous protein sequences were identified. After the syntheses of their codon-optimized genes, the synthetic genes have been cloned into a periplasmic expression vector to express in Escherichia coli. Among six homologous sequences, four sequences were successfully expressed in E. coli. The hydrolytic activities of the expressed proteins towards 4-nitrophenyl acetate and 4-nitrophenyl butyrate were measured and compared with those of CAL-B to identify whether the expressed proteins work as a hydrolase. It has been revealed that the expressed proteins can hydrolyze the substrates and the specific activities were determined as $(1.3-30){\times}10^{-2}{\mu}mol/min/mg$, which are lower than those of CAL-B. Among these homologous enzymes, Pseudozyma hubeiensis SY62 exhibits the comparable enantioselectivity to that of CAL-B towards the hydrolysis of (${\pm}$)-1-phenylethyl acetate.

Syntheses and Surface Active Properties of Amphoteric Surfactant Derivatives(5) - Basic Properties of Derivatives from Imidazoline (양쪽성 계면활성제의 유도체합성 및 계면성에 관한 연구(제5보) - 이미다졸린으로부터 유도된 유도체의 기초적 물성 -)

  • Ro, Y.C.;Kim, T.Y.;Jeong, J.K.;Nam, K.D.
    • Applied Chemistry for Engineering
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    • v.7 no.2
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    • pp.215-220
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    • 1996
  • Nine kinds of amphoteric surfactants were derived from 1-(2-hydroxyethyl)-2-undecyl-2-imidazoline. Their surface activities including surface tension and isoelectric points were measured in aqueous solution and critical micelle concentration(cmc) was also evaluated by the measurement of surface tension. From the measurement of surface tension, carboxylated amides revealed to be 26~40dyne/cm at $4.0{\times}10^{-4}{\sim}1.0{\times}10^{-3}mol/{\ell}$, sulfonated or sulfated imidazolines, 30~35 dyne/cm at $1.5{\times}10^{-3}{\sim}2.5{\times}10^{-3}mol/{\ell}$ and sulfonated amides, 25~33 dyne/cm at $5.8{\times}10^{-4}{\sim}8.0{\times}10^{-4}mol/{\ell}$ concentration range. It was found that isoelectric points of carboxylated amides were pH 7.2~7.9 and those of sulfonated or sulfated imidazolines and sulfonated amides were pH 4.5~5.5.

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Syntheses of New Lactones Containing Phenyl or Methyl Groups (페닐기 및 메틸기를 포함하는 새로운 lactone의 합성)

  • Chang, Seung Hyun;Moon, Sang Chil;Kim, Hak Hee;Lee, Kap Duk;Chung, Kwang Bo
    • Applied Chemistry for Engineering
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    • v.9 no.6
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    • pp.842-845
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    • 1998
  • Four new lactones and one dibenzo crown ether were synthesized by reaction of dihydroxy compound with oxalyl chloride and with ${\alpha}$,${\omega}$-dibromo compound, respectively. 5,6,11,12-Tetracarbonyl-2,2,3,3,8,8,9,9-octaphenyl-1,4,7,10-tetraoxacyclodode- cane(1), 5,6,11,12-tetracarbonyl-2,2,3,3,8,8,9,9-octamethyl-1,4,7,10-tetraoxacyclododecane(2), 7,8,15,16-tetracarbonyl-1,6,9,14-tetraoxacylclohexadecane(3), and 5,6,11,12-tetracarbonyl- 2,3,8,9- tetraphenyl-1,4,7,10-tetraoxacyclododecane(4) were prepared by reaction of oxalyl chloride with benzopinacol, pinacol, 2,2'-dihydroxybiphenyl and hydrobenzoin, respectively, in the presence of pyridine. Dibenzo-13-crown-4 (5) was obtained by reaction of catechol with 1,3-dibromopropane/1,2-dibromoethane.

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Chemical Modification of Nucleic Acids toward Functional Nucleic Acid Systems

  • Venkatesan, Natarajan;Seo, Young-Jun;Bang, Eun-Kyoung;Park, Sun-Min;Lee, Yoon-Suk;Kim, Byeang-Hyean
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.613-630
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    • 2006
  • Nucleic acids are virtually omnipresent; they exist in every living being. These macromolecules constitute the most important genetic storage material: the genes. Genes are conserved throughout the evolution of all living beings; they are transmitted from the parents to their offspring. Many interdisciplinary research groups are interested in modifying nucleic acids for use in a wider variety of applications. These modified oligonucleotides are used in many diverse fields, including diagnostics, detection, and therapeutics. In this account, we summarize our research efforts related to modified nucleic acid systems. First, we discuss our syntheses of modified oligonucleotides containing fluorescent tags for use as molecular probes (molecular beacons) to detect single-nucleotide polymorphisim (SNP) in nucleic acids and to distinguish between the B and Z forms of DNA. We also describe our research efforts into oligonucleotides functionalized with steroid derivatives to enhance their cell permeability, and the synthesis of several calix[4]arene-oligonucleotide conjugates possessing the ability to form defined triplexes. In addition, we have performed systematic studies to have an understanding about the functional groups necessary for a given nucleoside to behave as an organo or hydrogelator. The aggregation properties of a number of nucleoside-based phospholipids have been examined in different solvents; some of these derivatives are potential candidates for use as nucleoside-based liposomes. Finally, we also describe our research efforts toward the preparation of isoxazole- and isoxazoline-containing nucleoside derivatives and the determination of their antiviral activities.

Syntheses and Characterization of Cr(III)-Hydrogensalicylato and -Hydroxonitrophenolato Tetraaza Macrocyclic Complexes

  • Byun, Jong-Chul;Yoon, Chang-Hoon;Mun, Dae-Hun;Kim, Ki-Ju;Park, Yu-Chul
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.687-693
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    • 2006
  • Chromium(III) complexes, cis-[Cr([14]-decane)$(HOC _6H _4COO) _2$]$ClO _4$ I and cis-[Cr([14]-decane)(OH) $(OC _6H _4NO _2)$]$ClO _4{\cdot}H _2O$ II ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) are synthesized and structurally characterized by a combination of elemental analysis, conductivity, IR and VIS spectroscopy, and X-ray crystallography. The complexes crystallizes in the monoclinic space groups, $C2 _1$/a in I and $P2 _1$/n in II. Analysis of the crystal structure of complex I reveals that central chromium(III) ion has a distorted octahedral coordination environment and two hydrogensalicylato ligands are unidentate to the chromium(III) ion via the carboxyl groups in the cis-position. For monomeric complex I the hydrogensalicylato coordination geometry is as follows: Cr-O(average) = 1.984(3) $\AA$;Cr-N range = 2.105(3)-2.141(4) $\AA$;C(24)-O(4) = 1.286(5) $\AA$;N(2)-Cr-N(4) (equatorial position) = 96.97(15)${^{\circ}}$; N(1)-Cr-N(3) (axial position) = 168.27(15)${^{\circ}}$; O(1)-Cr-O(4) = 85.70(13)${^{\circ}}$. The crystal structure of II has indicated that chromium(III) ion is six-coordinated by four secondary amines of the macrocycle, hydroxide anion and nitrophenolate anion.

Novel Syntheses of 5-Aminothieno[2,3-c]pyridazine, Pyrimido[4',5':4,5]thieno[2,3-c]pyridazine, Pyridazino[4',3':4,5]thieno-[3,2-d][1,2,3]triazine and Phthalazine Derivatives

  • El Gaby, Mohamed S.A.;Kamal El Dean, Adel M.;Gaber, Abd El Aal M.;Eyada, Hassan A.;Al Kamali, Ahmed S.N.
    • Bulletin of the Korean Chemical Society
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    • v.24 no.8
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    • pp.1181-1187
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    • 2003
  • Condensation of 4-cyano-5,6-dimethyl-3-pyridazinone 1 with aromatic aldehydes gave the novel styryl derivatives 2a-c. Refluxing of compound 2a with phosphorus oxychloride furnished 3-chloropyridazine derivative 3. Compound 3 was reacted with thiourea and produced pyridazine-3(2H)thione 4. Thieno[2,3-c]- pyridazines 5a-e were achieved by cycloalkylation of compound 4 with halocompounds in methanol under reflux and in the presence of sodium methoxide. Also, refluxing of compound 4 with N-substituted chloroacetamide in the presence of potassium carbonate afforded thienopyridazines 6a-e. Cyclization of compound 6 with some electrophilic reagents as carbon disulfide and triethyl orthoformate furnished the novel pyrimido[4',5':4,5]thieno[2,3-c]pyridazines 12 and 13a-c, respectively. Diazotisation of compound 6 with sodium nitrite in acetic acid produced the pyridazino[4',3':4,5]thieno[3,2-d][1,2,3]triazines 14a-c. Ternary condensation of compound 1, aromatic aldehydes and malononitrile in ethanol containing piperidine under reflux afforded the novel phthalazines 16a-c. Compound 3 was subjected to some nucleophilic substitution reactions with amines and sodium azide and formed the aminopyridazines 17a, b and tetrazolo[1,5-b]-pyridazine 19, respectively. The structures of the synthesized compounds were established by elemental and spectral analyses.

Syntheses of New Nitrogen-Oxygen Multidentate Ligands and Their Stability Constants of Transition Metal(Ⅱ) Ions (새로운 질소-산소계 여러 자리 리간드의 합성 및 전이금속(Ⅱ)이온 착물의 안정도상수)

  • Kim, Sun Deuk;Jang, Ki Ho;Kim, Jun Kwang
    • Journal of the Korean Chemical Society
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    • v.42 no.5
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    • pp.539-548
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    • 1998
  • Multidentate N,O-containing ligands, such as N,N'-bis(2-hydroxybenzyl)-ethylenediamine(BHED), N,N'-bis(2-hydroxybenzyl)-propylenediamine(BHPD), N,N'-bis(2-hydroxybenzyl)-diethylenetriamine(BHDT), N,N'-bis(2-hydroxybenzyl)-triethylenetriamine(BHTT) and N,N'-bis(2-hydroxybenzyl)-tetraethylenepentaamine (BHTP) were synthesized by reduction of the imine group of Bis(salicylidene)-ethylendiamine(BSED), Bis (salicylidene)-propylenediamine(BSPD), Bis(salicylidene)-diethylentriamine(BSDT), Bis(salicylidene)-triethylenetetraamine(BSTT) and Bis(salicylidene)-tetraethylenepentaamine(BSTP). Proton dissociation constants of the ligands and stability constants of transition metal(Ⅱ) ion complexes with BHED, BHPD, BHDT, BHTT, and BHTP were determined by potentiometic titration. The sequence of stability constants $(logK_{ML})$ of complex increases as BHED Zn(Ⅱ) which follows the Irving-Williams series.

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Asymmetric Sythesis of Unnatural L-Amino Acids Using Thermophilic Aromatic L-Amino Acid Transaminase

  • Cho, Byung-Kwan;Seo, Joo-Hyun;Kim, Ju-Han;Lee, Chang-Soo;Kim, Byung-Gee
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.11 no.4
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    • pp.299-305
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    • 2006
  • Aromatic L-amino acid transaminase is an enzyme that is able to transfer the amino group from L-glutamate to unnatural aromatic ${\alpha}-keto$ acids to generate ${\alpha}-ketoglutarate$ and unnatural aromatic L-amino acids, respectively. Enrichment culture was used to isolate thermophilic Bacillus sp. T30 expressing this enzyme for use in the synthesis of unnatural L-amino acids. The asymmetric syntheses of L-homophenylalanine and L-phenylglycine resulted in conversion yields of >95% and >93% from 150 mM 2-oxo-4-phenylbutyrate and phenylglyoxylate, respectively, using L-glutamate as an amino donor at $60^{\circ}C$. Synthesized L-homophenylalanine and L-phenylglycine were optically pure (>99% enantiomeric excess) and continuously pre-cipitated in the reaction solution due to their low solubility at the given reaction pH. While the solubility of the ${\alpha}-keto$ acid substrates is dependent on temperature, the solubility of the unnatural L-amino acid products is dependent on the reaction pH. As the solubility difference between substrate and product at the given reaction pH is therefore larger at higher temperature, the thermophilic transaminase was successfully used to shift the reaction equilibrium toward rapid product formation.