• Title/Summary/Keyword: A new reagent

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Selective Reduction of Organic Compounds with Al-Trifluoromethanesulfonyldiisobutylalane. Comparison of Its Reactivity with Al-Methanesulfonyldiisobutylalane

  • Cha, Jin-Soon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.219-224
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    • 2011
  • The new MPV type reagent, Al-trifluoromethanesulfonyldiisobutylalane ($DIBAO_3SCF_3$), has been prepared and its reducing characteristics in the reduction of selected organic compounds containing representative functional groups have been examined, and compared its reactivity with that of Al-methanesulfonyldiisobutylalane ($DIBAO_3SCH_3$) in order to understand the fluorine-substituent effect on its reactivity. In general, the reactivity of $DIBAO_3SCF_3$ appears to be much higher than that of $DIBAO_3SCH_3$, apparently due to the acidity increase by the electron-withdrawing fluorine-substituent. The reagent reduced aldehydes and ketones readily, but showed a perfect selectivity in the reduction of $\alpha,\beta$-unsaturated aldehydes and ketones to produce the corresponding allylic alcohols in an absolutely 100% purity. In addition, the reagent achieved the regioselective cleavage of phenyl- or/and alkyl-substituted epoxides to the less substituted alcohols in a perfect regioselectivity. Moreover, the reagent also showed an high stereoselectivity in the reduction of substituted cycloalkanones to produce the thermodynamically more stable alcohol epimers exclusively.

Development of a New Method for Total Isocyanate Determination Using the Reagent 9-Anthracenylmethyl 1-Piperazinecarboxylate(PAC):Part 1 - The reaction condition and stability (9-Anthracenylmethyl 1-Piperazinecarboxylate(PAC)을 이용한 공기중 총이소시아네이트 분석방법 개발:제1부 반응조건 및 안전성)

  • Roh, Young-Man;Streicher, Robert P.
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.9 no.2
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    • pp.167-176
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    • 1999
  • A new analytical procedure for the measurement of monomeric isocyanates and total isocyanate group in workplaces has been investigated. The method described herd involves derivatization of the isocyanate sample upon collection with the reagent 9-anthracenylmethyl 1-piperazinecarboxylate (PAC). Laboratory investigations have demonstrated that excess PAC reagent can be satisfactorily removed from PAC-derivatized monomeric isocyanates-a requirement for the success f the analytical procedure. After removal of excess PAC reagent, the PAC derivatives of butyl isocyanate, phenyl isocyanate, HDI, MDI, and TDI were reacted with sodium thiomethoxide to convert them all to 9-anthracenylmethyl methyl sulfide (AMMS). Total isocyanate group was determined by HPLC analysis and quantification of the single AMMS peak. This circumvents many of the disadvantages associated with current HPLC methods. There were no longer problems associated with quantifying late-eluting peaks and analysis times were very short. A single detector was used for quantification because a standard of the analyte existed and the retention time could be determined. Because all species were converted to a single analyte, the problem of variability of response factors among different species was averted. Finally, there were no complex chromatograms to interpret. Monomers of other individual species were measured by analysis of the sample before the individual species were converted to AMMS. The favorable performance of PAC warrants its further study as a reagent for the determination of total isocyanate group in air.

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A Simple Device of the Dry Tetrabromophenolphthalein Ethyl Ester Reagent Strip for the Detection of Methamphetamine

  • Choi, Myung-Ja;Song, Eun-Young;Kim, Seung-Ki;Choi, Jeong-Eun;Lho, Dong-Seok;Park, Jong-Sei
    • Archives of Pharmacal Research
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    • v.16 no.3
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    • pp.227-230
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    • 1993
  • A new device to detect methamphetamine (MA), amphetamine(A) and its metabolites in urine was developed using the paper strip method and the test tube method of dry chemical reagents. The reagent containing tetrabromophenolphthalein ethyl ester (TBPE) and borax. For the TBPE paper strip method, a device was prepared with a window at each end of the reagent paper strip ; one window is for the sample application, and the other window is for the methylene chloride. The diffused sample from one window reacts with reagent in the paper and produces color at the point where it meets with methylene chloride which has diffused form the other side. A positive smaple produces as red-purple color and the negative sample a greenish color, with a detection limit of 5-10 ppm. The result can be obtained within one minute. For the TBPE test tube method which contains dry reagents, the detection limit is 5 ppm and the result can be obtaineed within 30 seconds, however the carry-on is not as convenient as the paper strip method. The performance of both methods were evlauated by comparing with the results of gas chromatography (GC) and fluorescence polarizaiton immunoassay (FPIA). The results were proven that both methods were useful as primary screening reagents to detect MA in urine and in dry powder.

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Peroxide Constituents in the Natural Product Research (천연물 연구에서의 Peroxide 성분)

  • Lee, Kang-Ro
    • Korean Journal of Pharmacognosy
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    • v.22 no.3
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    • pp.145-155
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    • 1991
  • Peroxides in natural products have been recently received a considerable attention due to their various biological and pharmacological properties. Nearly 300 peroxides have been isolated and structually characterized from natural sources, mainly as constituents of Compositae and marine sponge, and occur randomly in about 10 other plant families. Among peroxides studied, sesquiterpene endoperoxide, quinghaosu, has been already clinically applied as a new antimalarial drug. Based on the peroxides reported, structural classification, natural distribution and biological and pharmacological activities are reviewed. Color reagent and spectroscopic identification of peroxide are also described.

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Preconcentration and Determination of Fe(III) from Water and Food Samples by Newly Synthesized Chelating Reagent Impregnated Amberlite XAD-16 Resin

  • Tokahoglu, Serife;Ergun, Hasan;Cukurovah, Alaaddin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1976-1980
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    • 2010
  • A simple and reliable method has been developed to selectively separate and concentrate trace amounts of Fe(III) ions from water and food samples by using flame atomic absorption spectrometry. A new reagent, 5-hydroxy-4-ethyl-5,6-di-pyridin-2-yl-4,5-dihydro-2H-[1,2,4] triazine-3-thione, was synthesized and characterized by using FT-IR spectroscopy and elemental analysis. Effects of pH, concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of Fe(III) were investigated. The optimum pH was found to be 5. Eluent for quantitative elution was 10 mL of 2 M HCl. The preconcentration factor of the method, detection limit (3s/b, ${\mu}gL^{-1}$) and relative standard deviation values were found to be 25, 4.59 and 1%, respectively. In order to verify the accuracy of the method, two certified reference materials (TMDA 54.4 lake water and SRM 1568a rice flour) were analyzed. The results obtained were in good agreement with the certified values. The method was successfully applied to the determination of Fe(III) ions in water and food samples.

UV-HPLC Determination of Carbowyl Group Using 2-Bromoacetyltriphenylene as a Pre-labeling Reagent - The isolative determination of prostaglandin $E_2$ and $F_2{\alpha}$ by HPLC (2-Bromoacetyltriphenylene 유도체화제를 이용한 카르복실기 함유성분의 분석법 (I) - 프로스타글란딘 $E_2$$F_2{\alpha}$ 혼합물의 HPLC에 의한 분리정량)

  • 이왕규;정해수;김박광
    • YAKHAK HOEJI
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    • v.30 no.6
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    • pp.311-316
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    • 1986
  • A new UV labeling reagent was developed and used in HPLC for the determination of prostaglandin $E_2$ which have weak UV light-absorbing property. This reagent, 2-bromoacetyltriphenylene, was synthesized by the bromination of 2-acetyltriphenylene which was obtained from triphenylene by Friedel-Crafts reaction. The wave length maximum (${\lambda}_{max}^{CH_3CN}$ of this reagent was 268nm. Prostaglandin E$_2$ was extracted from prostaglandin E$_2$-$\beta$-cyclodextrin using a Sep-pak $C_{18}$ cartridge. The prostaglandin E$_2$ was labeled with 2-bromoacetyl-triphenylene in aectonitrite using 18-crown-6-ether as catalyst. Derivatized prostaglandins were separated on a reversed-phase column (Radial-pak) $\mu$-Bondapak $C_{18}$ using acetonitrile: water=60:40 as mobile phase. The effluent was monitored by UV detector at 254nm filter kit. Linearity of calibration curve was obtained between 30ng and 140ng, and the lower limit of detection was 5ng.

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Preparation and Characterization of Pore-filled Membrane Based on Polypropylene with Poly(vinylbenzyl chloride) by Using in-situ Cross-linking Technique

  • Kwon, Byeong-Min;Ko, Moon-Young;Hong, Byung-Pyo;Byun, Hong-Sik
    • Korean Membrane Journal
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    • v.10 no.1
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    • pp.13-19
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    • 2008
  • Water softening is a very promising field for membranes and especially ultra low pressure membranes. Nanofiltration membranes based on pore-filling technology was prepared by using a new technique: the in-situ cross-linking. This route involves introducing a pre-formed polymer into the pores of a host membrane and then locking the polymer in the pores by in-situ cross-linking with an appropriate reagent. By this way, it is possible to make robust and competitive, pore-filled, anion-exchange membranes with excellent control over the properties of the incorporated gel without affecting the host membrane. In this paper, the possibilities of tuning such membranes for ultra low pressure water softening was examined by altering pore-filling chemistry (by changing cross-linking and aminating reagents). The results showed that tuning the chemistry of the pore-filling has important effects. In particularly, it had been shown that the correct selection of cross-linking reagent was not only essential to get pore-filled membranes but it could control their properties. Moreover, the aminating reagent could improve membrane performance. It was found that an increase in hydrophobicity could improve the Darcy permeability.