• Title/Summary/Keyword: DBU

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Determination of Carboxyl Drugs by Gas Chromatography-Flame Photometric Detector (가스크로마토그라피-염광광도 검출기에 의한 혈장중 카르복실기 함유 약물의 정량)

  • 박만기;조영현;유무영;강탁림
    • YAKHAK HOEJI
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    • v.30 no.4
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    • pp.180-184
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    • 1986
  • Such carboxyl drugs as mefenamic acid, alclofenac, ketoprofen, cicloxilic acid and tolfenainic acid in rat plasma were determined by the gas chromatography flame photometric detector (GC-FPD). After methylthiomethyl (MTM) esterification with MTM-chloride in 1, 8-diazabicyclo [5.4.0] undec-7-ene (DBU) catalyst, determination of these drugs by this method was tried and compared with that by the GC-flame ionization detector (FID) method in respect to sensitivity and effect of inteferences. The results showed it was possible to analyze with accuracy by this method because of specificity of the FPD, although these drugs were not separated from interferences in plasma on GC column. The GC-FPD method was more sensitive than GC-FID method and the minimum detectable amount of monocarboxylic drugs on 3%, QF-1 column was about 15fmol/injection.

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Novel Syntheses of Isomers of Damascenone from Ethyl 2,6,6-Trimethyl-4-oxo-2-cyclohexene-1-carboxylate

  • Lee, Woo-Young;Jang, Se-Young;Lee, Jun-Gu;Chae, Woo-Ki
    • Bulletin of the Korean Chemical Society
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    • v.12 no.1
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    • pp.31-35
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    • 1991
  • Three isomers of damascenone, odorous terpenic ketones, have been synthesized conveniently from a same starting material, ethyl 2,6,6-trimethyl-4-oxo-2-cyclohexene-1-carboxylate(1), which was easily available by the acid-catalyzed condensation of mesityl oxide or acetone with ethyl acetoacetate. ${\alpha}$-Damascenone(7) was prepared by converting the enone ester 1 into the corresponding tosylhydrazone(4), followed by treating with 4 molar equiv of allyllithium. ${\beta}$-Damascenone(12) was synthesized by chemoselective reduction of 1 with sodium borohydride/cerium chloride to give corresponding allylic alcohol 8, conversion of 8 into acetate 9, and thermal decomposition of 9 with DBU to afford ethyl ${\beta}$-safranate(10), followed by reaction with an excess amount of allyllithium. ${\gamma}$-Damascenone(15) was obtained by dehydration of 8 with boric acid to furnish ${\gamma}$-safranate(13), followed by treatment with 2 molar equiv of allyllithium.

A Kinetic Study of Biphenyl Type Epoxy-Xylok Resin System with Different Kinds of Catalysts

  • 한승;김환근;윤호규;문탁진
    • Bulletin of the Korean Chemical Society
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    • v.18 no.11
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    • pp.1199-1203
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    • 1997
  • The investigation of cure kinetics of biphenyl epoxy (4,4-diglycidyloxy-3,3,5,5-tetramethyl biphenyl)-xylok resin system with four different catalysts was performed by differential scanning calorimeter using an isothermal approach. All kinetic parameters of the curing reaction including the reaction order, activation energy and rate constant were calculated and reported. The results indicate that the curing reaction of the formulations using triphenylphosphine (TPP) and 1-benzyl-2-methylimidazole (1B2MI) as a catalyst proceeds through a first order kinetic mechanism, whereas that of the formulations using diazabicyloundecene (DBU) and tetraphenyl phosphonium tetraphenyl borate (TPP-TPB) proceeds by an autocatalytic kinetic mechanism. To describe the cure reaction in the latter stage, we have used the semiempirical relationship proposed by Chern and Poehlein. By combining an nth order kinetic model or an autocatalytic model with a diffusion factor, it is possible to predict the cure kinetics of each catalytic system over the whole range of conversion.