• 제목/요약/키워드: Triethylamine

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Chiral Separation of Tryptophan by Immobilized BSA(bovine serum albumin) Membrane (BSA고정막에 의한 Tryptophan 이성질체의 분리)

  • Kim Min;Kim Jae-Hun;Na Won-Jae;Kim Byoung-Sik
    • Membrane Journal
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    • v.16 no.2
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    • pp.133-143
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    • 2006
  • A hollow fiber membrane containing BSA as ligand was Prepared by radiation-induced grafting GMA onto a porous polyethylene hollow fiber and subsequent reacting with DEA and TEA. The density of the DEA and TEA of the membrane were 3.4 mmol/g, 1.7r mmol/g, respectively. The DEA membrane exhibited a higher amount of than the TEA membrane. BSA was immobilized by the graft chains during the permeation of BSA solution throught the DEA and TEA membrane. The BSA was adsorbed in multilayer binding of 8 onto the DEA membrane whereas adsorption onto the TEA membrane remained constant. A two-stage stepwise BTC was observed due to independent chiral recognition for L, D-Trp solution by DEA-BSA membrane.

Synthesis and Characterization of New Polyaza Macrocyclic Nickel(Ⅱ) and Copper(Ⅱ) Complexes Two Nitrile or Imidate Ester Pendant Arms: Metal-Mediated Hydrolysis and Alcoholysis of the Nitrile Groups

  • Kang, Shin-Geol;Song, Jeong-Hoon;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.23 no.6
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    • pp.824-829
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    • 2002
  • New di-N-cyanomethylated tetraaza macrocycle 2.13-bis(cyanomethyl)-5.16-dimethyl-2,6,13,17-tetraazatricyclo[$16.4.0.0^7.12$]docosane $(L^2)$ has been prepared by the reaction of 3, 14-dimethyl-2,6,13,17-tetraazatricyclo $(L^1)$ with bromoacetonitrile. The square-planar complexes $[ML^2](ClO_4)_2(M=Ni(II)$ or Cu(II) can be prepared by the reaction of $L^2$ with the corresponding metal ion in acetonitrile. The cyanomethyl groups of $[ML^2](ClO_4)_2readily$ react with water to $yield[ML^3](ClO_4)_2$ containing pendant amide groups. The trans-octahedral complexes $[ML^4](ClO_4)_2$, in which two imidate ester groups are coordinated to the metal ion, can be also prepared by the reaction of $[ML^2](ClO_4)_2with$ methanol under mild conditions. The hydrolysis and alcoholysis reactions of $[ML^2](ClO_4)_2are$ promoted by the central metal ion, in spite of the fact that the cyanomethyl group is not involved in intramolecular coordination. The reactions are also promoted by a base such as triethylamine but are retarded by an $acid(HClO_4).Interestingly$, the imidate ester groups of $[ML^4]^2$ are unusually resistant to hydrolysis even in 0.1 M $HCIO_4$ or 0.1 M NaOH aqueous solution. Crystal structure of $[NiL^4](ClO_4)_2shows$ that the Ni-N (pendant imidate ester group) bond is rlatively strong; the Ni-N bond distance is shorter then the Ni-N(tertiary) distance and is similar to the Ni-N (secondary) distance.

Polyimide Multilayer Thin Films Prepared via Spin Coating from Poly(amic acid) and Poly(amic acid) Ammonium Salt

  • Ha, You-Ri;Choi, Myeon-Cheon;Jo, Nam-Ju;Kim, Il;Ha, Chang-Sik;Han, Dong-Hee;Han, Se-Won;Han, Mi-Jeong
    • Macromolecular Research
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    • v.16 no.8
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    • pp.725-733
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    • 2008
  • Polyimide (PI) multilayer thin films were prepared by spin-coating from a poly(amic acid) (PAA) and poly(amic acid) ammonium salt (PAAS). PI was prepared from pyromellitic dianhydride (PMDA) and 4,4'-oxydianiline (ODA) PAA. Different compositions of PAAS were prepared by incorporating triethylamine (TEA) into PMDA-ODA PAA in dimethylacetamide. PI multilayer thin films were spin-coated from PMDA-ODA PAA and PAAS. The PAAS comprising cationic and anionic moieties were spherical with a particle size of $20{\sim}40\;nm$. Some particles showed layers with ammonium salts, despite poor ordering. Too much salt obstructed the interaction between the polymer chains and caused phase separation. A small amount of salt did not affect the interactions of the interlayer structure but did interrupt the stacking between chains. Thermogravimetric analysis (TGA) showed that the average decomposition temperature of the thin films was $611^{\circ}C$. All the films showed almost single-step, thermal decomposition behavior. The nanostructure of the multilayer thin films was confirmed by X -ray reflectivity (XRR). The LF 43 film, which was prepared with a 4:3 molar ratio of PMDA and ODA, was comprised of uniformly spherical PAAS particles that influenced the nanostructure of the interlayer by increasing the interaction forces. This result was supported by the atomic force microscopy (AFM) data. It was concluded that the relationship between the uniformity of the PAAS particle shapes and the interaction between the layers affected the optical and thermal properties of PI layered films.

Synthesis and Characterization of Waterborne Polyurethane using Nano Zinc oxide (나노 산화아연을 사용한 수분산 폴리우레탄의 합성과 특성)

  • Cheon, Jung Mi;Jeong, Boo Yeong;Yoo, Chong Sun;Park, Duck Jei;Chun, Jae Hwan
    • Journal of Adhesion and Interface
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    • v.9 no.4
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    • pp.17-23
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    • 2008
  • In this study, waterborne polyurethane (WPU)/nano ZnO was synthesized from various polyester polyols, 4,4-dicyclohexylmethane diisocyanate ($H_{12}MDI$), dimethylolpropionic acid (DMPA), triethylamine (TEA) and ethylenediamine (EDA), nano ZnO. The contents of metal oxide were varied from 0 to 1.0 wt% of total solid. The effects of nano ZnO contents and ionic contents in the WPU/nano ZnO on thermal, mechanical properties were studied. The glass transition temperature ($T_g$) of WPU/nano ZnO do not show a distinct tendency with incorporation of nano ZnO and the $T_g$ of WPU/nano ZnO a little increased with increase of DMPA contents. The tensile strength and 100% modulus increase and elongation at break decreases with increase of nano ZnO contents and DMPA contents.

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High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Won-Woong;Lee, Sun-Young;Yu, Se Mi;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3727-3734
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    • 2012
  • An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.

HPLC Separation of Isoquinoline Alkaloids for Quality Control of Corydalis species

  • Kim, Eun-Kyung;Jeong, Eun-Kyung;Han, Sang-Beom;Jung, Jee-H.;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3597-3602
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    • 2011
  • A simple and rapid analytical method was developed for the determination of eight isoquinoline alkaloids in Corydalis species. Eight isoquinoline alkaloids, including 2 aporphine alkaloids (isocorydine and glaucine) and 6 protoberberine alkaloids (coptisine, palmatine, berberine, canadine, corydaline, and tetrahydrocoptisine) were used as chemical markers which have a various biological activity and determined for quality control of Corydalis (C.) species (C. ternata, C. yanhusuo, and C. decumbens). To evaluate the quality of these herbal medicines, LC chromatographic separation of alkaloids were preferentially investigated on reversed-phase C18 column with pH variation and composition of mobile phase. In addition, the separation of these alkaloids in herbal extracts was found to be significantly affected on mobile phase composition using gradient elution. Especially for C. yanhusuo extract, berberine was seriously interfered with other alkaloid extracted from sample matrix when mobile phase composition was not optimized. As results, these compounds were successfully separated within 28 min using 10 mM ammonium acetate containing 0.2% triethylamine (adjusted at pH 5.0) as a mobile phase with gradient elution. On the basis of optimized HPLC conditions, 23 different Corydalis species samples were analyzed for the determination of alkaloid levels. In addition, principal component analysis (PCA) combined with the chromatographic data could be successfully classified the different geographic origin samples.

Synthesis of Indoline tri-isopropyl benzene sulfonamide as a potential new asymmetric catalyst (새로운 술폰아미드계의 촉매의 합성)

  • Yun, In-Gwon;Kim, Hwan-Cheol
    • The Journal of Natural Sciences
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    • v.7
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    • pp.47-51
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    • 1995
  • In order to develope new asymmetric catalyst, we synthesized the following new sulfonamide derivatives start from S-Indoline-2-Carboxylic Acid via the following 5 steps. Hydroxy methyl derivative(1) was thus treated with methane sulfonyl chloride in the presence of triethylamine as base to give mesylated derivative(2) in 85% of isolated yield. The mesylate compound (2) was treated with excess sodium azide to give Azido derivative (4) in 95% isolated yield. Azido compound (3) was then reduced to the corresponding amino derivative in near quntitative yield by the hydrogenation under hydrogen atmospere in the presence of catalytic amount of Pd-C. The amino derivative (4) was converted to its sulfonamide derivatives by the treatment of compound(4) with triisopropyl benzene sulfonyl chloride in the presence of triethyl amine as base. Finally t-BOC group of the compound(5) was removed by the treatement of excess Trifluoro-acetic acid in near quantitative yield to give the target sulfonamide derivative (7) .in this paper we prepared compound(6) in 49% overall yield via the 5 steps of synthesis starting from t-Boc- 2-hydroxy methyl indoline(1) which cab be easily prepared from commercial available S-indoline-2-carboxylic acid by known methods. we plan to apply this new catalyst for the asymmetric reduction , diels-alder reaction, aldolcondensation reaction in due courses.

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Synthesis of Conjugated Dienals by Palladium-Catalyzed Vinyl Substitution Reaction (팔라듐 촉매화 비닐 치환 반응을 이용한 Conjugated Dienals의 합성)

  • Jong-Tae Lee;Jin Il Kim
    • Journal of the Korean Chemical Society
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    • v.28 no.5
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    • pp.335-341
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    • 1984
  • Acetals of ${\alpha},{\beta}$-unsaturated aldehydes reacted readily with aryl bromides in the presence of palladium catalyst and triethylamine to form aryl conjugated enals. Acrolein diethyl acetal and methacrolein diethyl acetal were reacted with phenyl bromides with substituents such as methyl and isopropyl groups at $100^{\circ}C$. The reaction products yields except the reaction of o-bromotoluene with methacrolein diethyl acetal. The products were identified by proton nuclear magnetic resonance and infrared spectroscopy. In the reverse combination of reactants to prepare aliphatic 2,4-dienals in good yield of above 50%, 3-bromopropenal dimethyl acetal and (E)-3-bromo-2-methylpropenal diethyl acetal were used as vinylic halide reactants and 1-alkenes and ethyl acrylate as olefin reactants.

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Determination of Ketorolac in Human Serum by High-performance Liquid Chromatography

  • Chun, In-Koo;Kang, Hyun-Hee;Gwak, Hye-Sun
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.529-534
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    • 1996
  • A high-performance liquid chromatographic (HPLC) assay has been developed for the determination of ketorolac in human serum using a new extraction method with a good recovery. Human serum samples (1.0 ml) spiked with known concentrations of ketorolac tromethamine and 10${\mu}g$ of ketoprofen as the internal standard (IS) were acidified with 200${\mu}l$ of 1 N HCl and extracted with 7 ml of n-hexane-ether (7:3 v/v). Extracts were centrifuged and organic layer was back-extracted with 400${\mu}l$ of 0.1% tromethamine solution. Twenty .mu.l of centrifuged aqueous layer was injected onto a reversed-phase octyl column and eluted with a mixture of acetonitrile, water, methanol, and triethylamine [35:55:10:0.1 (v/v), pH 3.0] at a flow rate of 1.0 ml/min. Ultraviolet detection of ketorolac and IS was carried out at 300 nm. The calibration curve obtained using peak area ratios showed a good linearity (in concentration range 10-150 ng/ml $r^2$=O.9944; in range 50-2000 ng/ml, r$^{2}$=0.9998). The mean intra-day accuracy and precision for this HPLC method were found to be 3.6 and 3.7%, respectively. The mean inter-day accuracy and precision were found to be 4.0 and 3.7%, respectively, in the concentration range 50-2000 ng/ml. The recovery of ketorolac from serum was 92.0 $({\pm}5.7)$ % at the concentration of 100 ng/ml. This method proved to be readily applicable to the assay of ketorolac in human serum.

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A Study on the Removal Efficiency of VOCs and Operating Characteristics by Using of Bioscrubber Trickling Filter(BSTE) (Bioscrubber Trickling Filter(BSTF)의 VOCs 제거 및 운전 특성에 관한 연구)

  • Park, Jin-Do;Suh, Jung-Ho;Lee, Hak-Sung
    • Journal of Environmental Health Sciences
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    • v.31 no.4 s.85
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    • pp.309-315
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    • 2005
  • Volatile organic compounds (VOCs) and odor materials are major sources of air pollution in Ulsan city, where much chemical plants are located. Therefore, it is necessary to develop a new reactor which can remove VOCs and odor materials effectively and be equipped at the end of pipe easily. A modified reactor (bioscrubber trickling filter, BSTF), which have both characteristics of biofilter and bioscrubber, was developed and tested on its reactivity with several VOCs using two types of media, fiber and activated carbon 4- ceramic(A/C). It was observed that the removal efficiencies of several types of VOCs such as acetaldehyde, ethylalcohol, butanol, diethylamine and triethylamine were up to $95\%$ when they had about 100 ppm of initial concentration and 80 seconds of residence time. Good attachment of microorganisms to both media, where it is thought the reaction efficiency can be determined according to the amount of microorganisms attachment, observed with scanning electron microscopy(SEM). Initial pressure drops of the packed bed with both media were 229 $mmH_2O/m$ at A/C column and 670 $mmH_2O/m$, respectively. However, maximum pressure drop of fiber column during the operation was over 1,647 $mmH_2O/m$. Therefore, it was thought that the fiber material would not suitable to use in the local plant as a packed bed media.