• 약학회지
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• 제35권4호
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• pp.288-294
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• 1991

A new fluorescent derivatizing reagent was developed to be used in HPLC for the trace determination of primary and secondary amines. This new reagent, 1-(N,N-dimethylamino)pyrene-6-sulfonyl chloride, was synthesized by the chlorination of sodium 1-(N,N-dimethylamino)pyrene-6-sulfonate which was obtained from 1-(N,N-dimethylamino)pyrene after sulfonation. Ephedrine and norephedrine were derivatized quantitatively by this reagent. The optimum conditions for the derivatization such as pH, reagent concentration, reaction time and reaction temperature ware examined. The structures of derivatives were identified by IR, $^{1}$H-NMR and MS methods. The fluorescence properties and the stability of the derivatives were examined. The derivatives were separated on silica column with an isocratic elution using the mixture of n-hexane and ethylacetate and monitored by fluorescene detector. Linear calibration curves were obtained and detection limits in a 10 $\mu$l injection volume were 5 picomole for ephedrine and norephedrine.

• 분석과학
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• 제36권1호
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• pp.1-11
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• 2023

A new, sensitive, and reliable flow injection methodology was investigated for the determination of lead ion (II) in vegetables' samples using a laboratory-prepared reagent 2-[(6-methoxy-2-benzothiazoly)azo]-4-methoxy phenol (6-MBTAMP). Infrared spectroscopy, UV-visible spectrophotometry, Energy dispersive X-ray spectroscopy (EDX), Elemental Analysis (CHN), nuclear magnetic resonance spectroscopy ¹HNMR, and ¹³CNMR techniques were used to characterize the reagent and lead (II) complex. The method is based on lead ion (II) reacting with the reagent (6-MBTAMP) in a neutral solution to produce a green-red complex with a maximum absorbance at 670 nm. The optimum conditions, such as flow rate, lead ion (II) volume, reagent volume, medium pH, reagent concentration, and reaction coil length were thoroughly examined. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.621 mg·L^-1 and 2.069 mg·L^-1 , respectively, while Sandell's sensitivity was determined to be 0.345 ㎍·cm^-2.

• Bulletin of the Korean Chemical Society
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• 제31권4호
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• pp.840-844
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• 2010

The new MPV type reagent, Al-methanesulfonyldiisobutylalane ($DIBAO_3SCH_3$), has been prepared and its reducing characteristics in the reduction of selected organic compounds containing representative functional groups have been examined in order to find out a new reducing system with high selectivity in organic synthesis. In general, the reagent is extremely mild, showing only reactivity toward aldehydes, ketones and epoxides. The reagent exhibits a unique reducing applicability in organic synthesis. Thus, the reagent can achieve a clean 1,2-reduction of $\alpha,\beta$-unsaturated aldehydes and ketones to produce the corresponding allylic alcohols in 100% purity. In addition, the reagent shows an excellent regioselectivity in the ring-opening reaction of epoxides. Finally, $DIBAO_3SCH_3$ shows a high stereoselectivity in the reduction of cyclic ketones to produce the thermodynamically more stable epimers exclusively.

• Bulletin of the Korean Chemical Society
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• 제34권10호
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• pp.2953-2958
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• 2013

A noble phenylsulfonyl reagent 8 having ${\alpha}$-oxo (cyanomethylene)triphenylphosphorane ylide subunit readily condensed with various alkyl halides under basic conditions to afford ${\beta}$-alkyl-${\alpha}$-oxo-${\beta}$-phenylsulfonyl (cyanomethylene)triphenylphosphorane ylides 9 in excellent yields. These sulfonyl ylides 9 were then reductively desulfonylated with $Na(Hg)/Na_2HPO_4$ in the presence of methanol to provide ${\alpha}$-keto (cyanomethylene)-triphenylphosphorane ylides 2' in good to excellent yields. Our new synthetic approach offers an expeditious access to various ${\alpha}$-keto (cyanomethylene)triphenylphosphorane ylides from alkyl halides utilizing a new phenylsulfonyl reagent as the key reagent under mild reaction conditions in good overall yields.

• 통합자연과학논문집
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• 제2권3호
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• pp.185-189
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• 2009

The new MPV-type reagent, Al-fluorodiisobutylalane (DIBAF), has been prepared and their reducing characteristics in the reduction of selected organic compounds containing representative functional groups have been examined in order to find out a new reducing system with unique applicability in organic synthesis. In general, the reagent is extremely mild, showing only reactivity toward aldehydes, ketones, and epoxides. The reagent achives a clean 1,2-reduction of enals to the corresponding allylic alcohols in a 100% purity, but shows no reactivity toward enones. The reagent also shows an excellent regioselective cleavage of substituted epoxides. In addition, DIBAF produces the thermodynamically more stable alcohol epimer in high stereoselectivity in the reduction of cyclic ketones.

• Bulletin of the Korean Chemical Society
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• 제25권8호
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• pp.1277-1279
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• 2004

• Archives of Pharmacal Research
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• 제11권2호
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• pp.134-138
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• 1988

Urine measurements by MNR were made for 25 persons including cancer and non-cancer patients. The aromatic proton signals of NMR wer observed much more often in cancer patients' urine than non-cancer patients' one. To compare the amount of the phenolic compounds excreted in urine between cancer and non-cancer patient, urine analysis by HPLC with UV detector was performed. Total peak area and major peak areas of cancer patients' urine wer emuch greater than those of non-cancer patients' one. To check the phenolic compound excreted in urine, a new jellied reagent named Gift reagent which was based on Millon's reagent, was developed for urine color reaction. When the reagent was tested, the sensitivity and specificity for urine samples of 69 persons including cancer and non-cancer patients were measured by 85.3% and 91.4%, respectively, indicating that the Gift reagent afford a possibility of cancer diagnosis.

• Bulletin of the Korean Chemical Society
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• 제17권11호
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• pp.1009-1018
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• 1996

A study on the application of vinyl radical cyclization via free radical allylation reaction in the synthesis of various carbocyclic compounds is described. In connection with this study, a new allyl transfer reagent, 2-bromo-3-(phenylthio)propene 1 is developed and it was shown that vinyl radical cyclization through free radical allylation reaction using reagent 1 provides a valuable approach to carbocyclic systems with a reactive exo-alkylidene moiety, which is advantageous for further transformations.

• Bulletin of the Korean Chemical Society
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• 제29권5호
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• pp.1079-1082
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• 2008

• 약학회지
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• 제9권1_2호
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• pp.18-22
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• 1965

A new organic reagent, 1-isonicotinoyl-2-furfurylidene hydrazine was synthesized from isonicotinic acid hydrazide and furfural, gives precipitate with copper(II), mercury(II) and argent(I), whereas, it gives a water soluble yellow complex with iron(III). Copper complex of the reagent is soluble in EtOH MtOH, pyridine, dioxane and dimethylformamide with green yellow coloration. The complex has a maximum absorption at 385 m.$\mu$ and molar ratio of copper; reagent was estimated as 1:1 by continuous variation method, slop method and chelate titration method. Molar extinction coefficient (9600) and apparant formation constant of this complex was spectrophotometrically determined. K=1.7 * $10^{7}$ (Babko's method) K=2.1 * $10^{7}$ (Anderson's method). This reagent reacted with copper so sensitive that it would be available for determination of Cu (II).