• Title/Summary/Keyword: Trifluoroacetyl

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Analysis of Trifluoroacetyl group in PVA-polyvinyltrifluoroacetate Copolymer by the Pyrolysis Gas Chromatography (열분해 기체크로마토그래피를 이용한 PVA-polyvinyltrifluoroacetate 공중합체중의 trifluoroacetyl 기의 정량)

  • Chae, Hee-Ju;Jo, Seong-Mu;Lyu, Hark-Soo;Nakajima, Toshinari
    • Journal of the Korean Chemical Society
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    • v.31 no.3
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    • pp.287-291
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    • 1987
  • The composite mole fraction of monomers in PVA-PVFAc copolymer could be calculated from the analysis of trifluoroacetyl group by the pyrolysis gas chromatography without breaking of C-F bonds in polymer. A linearity between trifluoroacetyl peak areas in pyrogram and sample weights was obtained within the range below 3mg. The data of trifluoroacetyl contents derived from gas chromatogram of copolymers with various D.S. were in good agreement with results by the Specific Ionmeter.

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Photochemical Synthesis of Aspartylphenylalanyl Methyl Ester (광 알킬화 반응에 의한 Aspartylphenylalanyl Methyl Ester의 합성)

  • Sang Chul Shim;Kyu Ho Chae
    • Journal of the Korean Chemical Society
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    • v.19 no.5
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    • pp.367-374
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    • 1975
  • Glycine residue in N-X-glycylphenylalanine methyl ester(X = trifluoroacetyl or acetyl) was converted into aspartic acid derivative by a photoalkylation reaction. The reaction was induced with 350 nm lamp using a combination of diacetyl/di-t-butyl peroxide (DBP) as the photoinitiator, and acetic anhydride as the alkylating agent. In the thermal reaction with DBP and acetic anhydride, the same alkylation reaction of the dipeptide was observed. From this thermal alkylation reaction the photoalkylation reaction is also thought to undergo via free radical mechanism.

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Mild Isomerative Opening of Tetrahydrofuranyl Subunits in Steroids Using TFAT (trifluoroacetyl trifluoromethanesulfonate): Application to Synthesis of C17-OH Rockogenin Acetate

  • Lee, Jong-Seok;Kim, Byung-Sook;Shin, Jun-Ho;Lee, Yeon-Ju;Shin, Hee-Jae;Lee, Hyi-Seung
    • Bulletin of the Korean Chemical Society
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    • v.33 no.1
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    • pp.76-82
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    • 2012
  • A novel and efficient tetrahydrofuranyl ring opening method was developed using the highly reactive TFAT reagent in the presence of an acid scavenger, 2,6-di-tert-butyl-4-methylpyridine. Various acid sensitive groups are compatible with the reaction condition, making it generally applicable to many tetrahydrofuranyl steroids. Moreover, it is a synthetic equivalent of 'Marker degradation' affording an efficient synthesis of C17-OH rockogenin acetate.

Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Synthesis and Biological Evaluation of 4-Phenyl-1-(indoline-5-sulfonyl)-2-imidazolone Derivatives as Potential Antitumor Agents

  • Park, Dongrak;Lee, Jungah;Hyunsook Hwang;Lee, Dugkeun;Sungjune Yoon;Yongho Chung;Sanghun Jung;Lee, Moonsun
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1997.04a
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    • pp.73-73
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    • 1997
  • A series of 4-phenyl-1-(indoline-5-sulfonyl)-2-imidazolone derivatives has been synthesized starting from 2-bromoacetophenone. Reaction of 2-aminoacetophenone obtained from 2-bromoacetophenon by Delepin synthesis and potassium cyanate affords 1,3-dihydro-4-phenyl-2-imidazolone. This key intermediate was treated with sodium hydride and N-trifluoroacetyl-indoline-5-sulfonylchloride, and trifluoroacetyl group was deprotected to give 4-Phenyl-1-(indoline-5-sulfonyl)-2-imidazolone. Various substituents were introduced on the nitrogen of indoline. Antitumor activity of this series of compound was evaluated by MTT method. Nearly all of the compounds showed broad-spectrum activity.

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Enantiomeric Separation of Methamphetamine Abused in Korea (우리나라에서 남용되는 메스암페타민의 거울상 이성질체분리)

  • Yoo, Young-Chan;Chung, Hee-Sun;Choi, Hwa-Kyung;Kim, Eun-Mi;Kim, Mi-Kyung;Kim, Sun-Choon
    • YAKHAK HOEJI
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    • v.41 no.3
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    • pp.277-282
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    • 1997
  • Methamphetamine, which is the most commonly abused drug in Korea, exists in terms of d-, l- isomers and a racemate(dl). d-Methamphetamine is a potent central nervous system stimulant, whereas l-Methamphetamine is sold freely as a nasal decongestant. In addition, methamphetamine appears in different ratios of optical isomers by the clandestine synthesis applied. In this study, enetiomeric separation of methamphetamines was estabilished to distinguish the chirality of methamphetamines trafficked and abused in Korea. A gas chromatograph/mass spectrometer(GC/MS) system equipped with an achiral capillary column is used to isolate the isomers of methamphetamine after (S)-N-(trifluoroacetyl)-l-prolyl(TFP) deravatization.After analyzing 10 illicit methamphetamine powders and 10 positive urine samples, following findings were found: d-Methamphetamine was well resolved from l-Methamphetamine by chromatographic separation of TFP derivatibes on DB-5 with retention time of 11.80 and 11.35 min respectively. The detection of d-Methamphetamine in all 10 powders and 10 urine samples proves that all methamphetamines abused in Korea are illegally manyfactured and administred.

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A Study on the Analysis of Pesticide Residue in Banana by GC/MSD (GC/MSD를 이용한 바나나 중에서의 잔류농약 분석법에 관한 연구)

  • 박성수;김동원
    • The Korean Journal of Food And Nutrition
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    • v.9 no.2
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    • pp.217-222
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    • 1996
  • We studied about analyzing carbamate pesticides, organochlorine, organophosphorus pesticides simultaneously using by GC/MSD. For this, instead of HPLC which is generally used in analyzing carbamate pesticides, GC was used and all hydrogen of -NH group in carbamate pesticides were substituted for trifluoroacetyl group which is stable at heat And eight pesticide resdidues were not detected in nine samples circulated in the city.

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Preparation of Trifluoroacetyl Chitosan Derivatives with Antiviral Activity (항바이러스 활성을 갖는 Trifluoroacetyl Chitosan 유도체의 제조)

  • Kim, Chun-Ho;Shin, Cha-Gyun;Shin, Kye-Sook;Son, Tae-il
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.599-602
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    • 1999
  • Chitosan was depolymerized by using nitrous acid. In order to synthesize new fluorinated chitosan oligomer(FCO) derivative, free amine groups of resulting low molucular weight chitosan oligomers were reacted with trifluoroacetic anhydride. The structure changes in the samples were conformed by using FT-IR, $^{1}H\;NMR$, $^{13}C\;NMR$ and $^{19}F\{^{1}H\}NMR$. Antiviral activity of FCO was studied by measuring DAN amounts of the replication viruses at 36 hr after the cells were infected with the viral solution containing FCO of various concentrations. The viral replications in the cells infected with the viral solution containing FCO were proportionally decreased with the FCO does, compared to those of the control groups, indicating that FCO efficiently inhibits viral infection. In particular, viral replication was decreased to 40% in the 1% FCO-treated cells.

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