• Title/Summary/Keyword: Trifluoroacetic acid

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Efficient Hydrogenation Catalysts of Ni or Pd on Nanoporous Carbon Workable in an Acidic Condition

  • Lee, Dong-Hwan;Kim, Hong-Gon;Kang, Min;Kim, Ji-Man;Lee, Ik-Mo
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.2034-2040
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    • 2007
  • Efficient catalytic systems, where Ni or Pd is introduced in a supporting material of nanoporous carbon, have been developed for a liquid-phase hydrogenation of carboxylic acids and ketones at room temperature. It has been found that the catalysts reliably show high activities and selectivities for the hydrogenation to alcohols even in acidic conditions, and the catalytic activities depend on the preparative method of catalysts, the hydrogen pressure, the agitation rate, and the catalytic species. The hydrogenation of carboxylic acids and ketones clearly shows that the reaction rate is affected by the electronic and the steric effects, and a plausible reaction mechanism using metal hydrides as catalytic species is proposed.

Facile Synthesis and Characterization of Poly(dialkoxy-p-phenylene 1,3,4-oxadiazole-alt-phenylene 1,3,4-oxadiazole)s

  • Kim, Hoon-Seok;Kang, Soon-Min;Do, Jung-Yun
    • Macromolecular Research
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    • v.16 no.4
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    • pp.360-366
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    • 2008
  • Poly(dialkoxyphenylene 1,3,4-oxadiazole)s were conveniently synthesized to compare their material properties of solvent solubility, thermal stability and molecular alignment with respect to alkyl chain length and meta/para-phenylene structure. All prepared polymers exhibited good solubility in co-solvents containing various volume levels of chloroform to trifluoroacetic acid. Meta-polymers showed slightly better solubility than para-polymers. All polymers produced were thermally stable up to $320^{\circ}C$. Photoluminescence of polymer films was observed with blue light emission at around 450 nm. X-ray diffraction patterns of all polymers indicated that they were composed of stacked molecular sheets with the same layer-to-layer distance of $3.4\;{\AA}$. However, side chain-to-side chain and main chain-to-main distances within the layers increased with increasing alkyl chain lengths. The meta-polymer chains were separated more than the para-polymer chains.

Study on analytical method of residual macrolide antibiotics in livestock products by LC/MS (LC/MS를 이용한 축산물 중 잔류 마크로라이드계 항생물질 분석법 연구)

  • 황래홍;윤은선;김연주;김동언;양윤모;이정학;이병동
    • Korean Journal of Veterinary Service
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    • v.25 no.3
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    • pp.221-227
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    • 2002
  • This study was carried out to confirm analytical method of residual macrolides in livestock products by LC/MS. 1. Macrolides were analyzed by LC/MS on XTerra C$\sub$18/ column with 0.1% TFA(trifluoroacetic acid)-methanol in a gradient mode as mobile phase, and that were identified by positive chemical ionization with selective ion monitoring at 50~1000 mass range. 2. Residual macrolides were extracted from tissue with acetonitrile, and the extract is purified with a Sep-pak C$\sub$18/ cartridge, and elute macrolides with 0.1M methanolic ammonium acetate. 3. The procedure confirms the presence of each macrolide at 50$\mu\textrm{g}$/kg in spiked sample.

Preparation of Branched Polystyrene Using Atom Transfer Radical Polymerization Techniques and Protection-Deprotection Chemistry

  • Kwark, Young-Je
    • Macromolecular Research
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    • v.16 no.3
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    • pp.238-246
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    • 2008
  • A new strategy using protection-deprotection chemistry was used to prepare branched polymers using the ATRP method only. Among the several monomers with different protecting groups, vinyl benzyl t-butyloxy carbonate (VBt-BOC) and 4-methyl styrene (4-MeSt) could be polymerized successfully to form backbones using the ATRP method in a controlled fashion. The protected groups in the backbones were converted to alkyl bromides and used as initiating sites for branch formation. The benzyl t-butyloxy carbonate groups in the backbones containing VBt-BOC units were first deprotected to benzyl alcohol by trifluoroacetic acid, then converted to benzyl bromide by reacting them with triphenylphosphine/carbon tetrabromide. The benzyl bromide groups in the backbones containing 4-MeSt units could be generated by bromination of the methyl groups using N-bromosuccinimide/benzoyl peroxide. The structures of the prepared polymers were well-controlled, as evidenced by the controlled molecular weight as well as the narrow and unimodal molecular weight distribution.

Quantitative determination of pseudoephedrine in human plasma by reversed-phase liquid chromatography-electrospray ionization mass spectrometry

  • Kim, Jin-Ki;Cho, Jung-Hye;Woo, Jong-Soo;Kim, Chong-Kook
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.394.2-394.2
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    • 2002
  • A sensitive and selective reversed-phase LC-ESI-MS method to quantitate pseudoephedrine in human plasma was developed and validated. Phenacetin was used as an internal standard. Samples were prepared simply by acetonitrile precipitation without an evaporation step. Chromatographic separation was achieved on a XTerra MS C18 column ($150{times}2.1$ mm I.D.. 3.5 $\mu\textrm{m}$ particles). using gradient elution with 0.5% (v/v) trifluoroacetic acid (TFA) in water and 0.5% (v/v) TFA in methanol at a flow-rate of 0.1 ml/min. (omitted)

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Determination of MDMA and MDA in 44 hair samples during 2002 to 2003

  • Han, Eun-Young;Yang, Won-Kyung;Lee, Jae-Sin;Park, Yong-Hoon;Kim, Eun-Mi;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.112.1-112.1
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    • 2003
  • The qualitative and quantitative analysis of MDMA and MDA in hair samples by GC/MS were reported. Hairs were collected from subjects aged 22-37 years, who were suspected of abusing MDMA. After washing with methanol, hair samples were cut into small pieces, extracted with methanol containing 1 percent hydrochloric acid for 20th, and the solution was evaporated. MDMA or MDA in the extract were determined by GC/MS using selected ion monitoring after derivatization with trifluoroacetic anhydride. (omitted)

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Determination of Enantiomeric Purity of (S)-(+)-Ibuprofen by $^1$H-NMR using (-)- Cinchonidine as a Chiral Solvating Agent

  • Lee, Jae-Yong;Seo, Sang-Hun;Kang, Jong-Seong;Kim, Kyeong-Ho
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.219.1-219.1
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    • 2003
  • $^1$H-NMR method for the determination of enantiomeric purity of (S)-(+)-ibuprofen was developed using (-)-cinchonidine as a chiral solvating agent. (S)-(+)-ibuprofen was prepared by optical resolution of racemic ibuprofen using preferential recrystallization method with (S)-(-)-${\alpha}$-methylbenzylamine and (R)-(-)-ibuprofen by semi-preparative chiral HPLC using chiral OD column and n-hexane/2-propanol/trifluoroacetic acid as a mobile phase. Several concentrations of synthetic mixture of (S)-(+)-ibuprofen and (R)-(-)-ibuprofen were added to the (-)-cinchonidine disolved in CDCl$_3$. (omitted)

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Bilin and Bilinone Chlorophyll Catabolite Content in the Hamamelidaceae Autumnal Leaves

  • Djapic, Nina
    • Natural Product Sciences
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    • v.28 no.1
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    • pp.18-26
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    • 2022
  • In order to facilitate the quantification in autumnal Hamamelidaceae leaves, a HPLC method was used for the determination of two chlorophyll catabolites and their isomers: bilin-type (1) and bilinone-type (2) ones. The separation was done on a RP-C4 column with a gradient solvent system of 0.1% trifluoroacetic acid aqueous-methanol at the flow-rate of 0.2 mL/min and detected at 244 nm. The quantity of bilin-type (1) and bilinone-type (2) chlorophyll catabolite isomers from ten species of Hamamelidaceae autumnal leaves methanol extracts: Corylopsis pauciflora, Corylopsis spicata, Forthergilla major, Hamamelis intermedia, Hamamelis japonicum, Hamamelis japonicum var. flavopurpurscens, Hamamelis virginiana, Parrotiopsis jacquemontiana, Parrotia persica and X Sycoparrotia semidecidua were from 0.85 mg/g ~ 57.50 mg/g for bilin-type isomers (1) and 3.40 mg/g ~ 49.30 mg/g for bilinone-type isomers (2). The results obtained gave insight in quantitative bilintype (1) and bilinone-type (2) chlorophyll catabolite composition of the Hamamelidaceae plant species autumnal leaves.

Application of Bayer-Villiger Reaction to the Synthesis of Dibenzo-18-crown-6, Dibenzo-21-crown-7 and Dihydroxydibenzo-18-crown-6

  • Utekar, Druman R.;Saman, Shriniwas D.
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.193-197
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    • 2014
  • Dibenzo-18-crown-6, dibenzo-21-crown-7 and dihydroxy dibenzo-18-crown-6 were synthesized by Bayer-Villiger oxidation strategy. Dibenzo-18-crown-6 and dibenzo-21-crown-7 could be synthesized through a three-step protocol starting from salicylaldehyde. Salicylaldehyde was reacted with bis-(2-chloroethyl)ether using $K_2CO_3$ in acetonitrile to link the two phenolic groups with the oxyethylene bridge followed by conversion of the formyl group to the hydroxy group via a Baeyer-Villiger reaction and finally linking the two phenolic group with appropriate oxyethylene bridge. The two target crown ethers were obtained in overall yield, 24% and 30%, respectively. This method has a great potential for synthesis of symmetrical as well as unsymmetrical dibenzo crowns with varying oxyethylene bridges. Baeyer-Villiger oxidation could be used to prepare dihydroxy derivative of dibenzo-18-crown-6 through acetylation of dibenzo-18-crown-6 followed by Baeyer-Villiger oxidation. The Baeyer-Villiger oxidation could be substantially accelerated using trifluoroacetic acid.

Fabrication of Cross-linked Nano-Fibrous Chitosan Membranes and Their Biocompatibility Evaluation

  • Nguyen, Thi-Hiep;Lee, Seong-Jin;Min, Young-Ki;Lee, Byong-Taek
    • Korean Journal of Materials Research
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    • v.21 no.2
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    • pp.125-132
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    • 2011
  • Fibrous chitosan membranes were fabricated as a substrate for skin applications using an electro-spinning process with different solvents and varying concentrations. Scanning electron microscopy (SEM) images confirmed that the formation of the chitosan fibrous membrane in trifluoroacetic acid was better than that in acetic acid. Fourier transform infrared spectroscopy showed that the chitosan fibers were cross-linked with glutaraldehyde, and that the cytotoxicity of the aldehyde groups was reduced by glycine and washing by NaOH and DI water. Chitosan cross-linked fibrous membranes were insoluble in water and could be washed thoroughly to wash away glycine and excess NaOH and prevent the infiltration of other water soluble bio-toxic agents using DI water. MTT assay method was employed to test the cytotoxicity of chitosan membranes during fabricating, treating and washing processes. After the dehydration of cell cultured chitosan membranes, cell attachment behavior on the material was evaluated using SEM method. Effect of the treatment processes on the biocompatibility of the chitosan membranes was shown by comparing of filopodium and lamellipodium of fibroblast cells on grown washed and unwashed chitosan fibrous membrane. The MTT assay and SEM morphology confirmed that the washed chitosan fibrous membrane increased cell attachment and cell growth, and decreased toxicity compared to results for the unwashed chitosan fibrous membrane.