• Archives of Pharmacal Research
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• 제24권2호
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• pp.100-104
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• 2001

Differential pulse polarographic(DPP) analytical procedure for the rifampicin antibiotic, which can be applied to monitor its synthetic process from the starting antibiotic of rifamycin B or rifamycin SV has been developed based on the electrochemical reduction of an azomethine group. Rifampicin exhibited a cathodic peak due to the azomethine group in the side chain of 3-[(4-methyl-1-piperazinyl)imino]methyl moiety and another cathodic peak due to the carbonyl group in rifamycin SV by DPP. The experimental peak potential shift of an azomethine reduction was -73 mV/pH in the pH range between 3.0 and 7.5, agreeing with involvement of 4 e-and 5 $H^5$ in its reduction. By the cyclic voltammetric(CV) studies, the azomethine and the carbonyl reductions in rifampicin were processed irreversibly on the mercury electrode. The plot of peak currents vs. concentrations of rifampicin ranging $1.0{\times}10^{-7} M~$1.0{\times}10^{-5} M yielded a straight line with a correlation coefficient of 0.9996. The detection limit was $1.0{\times}10^{-8} M with a modulation amplitude of 50 mV DPP has been successfully applied for the determination of rifampicin in the pharmaceutical preparations.

• Archives of Pharmacal Research
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• 제2권2호
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• pp.111-114
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• 1979

Diazepam was investigated in aqueous buffer media using pulsed rotation voltammetry. The dependence of half-wave potentials on pH indicated a two proton involvement in a two electron transfer reduction in the pH range 3-10. Dizaepam at micromolar concentration levels may be determined by measurement of the limiting difference current.

• 농약과학회지
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• 제4권2호
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• pp.69-71
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• 2000

5-(2,3-dihydro-2,2-dimethylbenzothiophene-7-yl)-2-(1-(alkoxyimino)butyl)-3-hydroxy-2-cyclohexene-1-one 유도체중 azomethine 질소 원자상 alkoxy (RO)-기들이 변화함에 따른 논과 밭 조건에서 살초활성을 측정하고 기질분자(S)의 구조와 살초 활성과의 관계 (SAR)를 검토하였다. 특히, i-propoxy-치환체, 5는 4kg/ha의 농도에서 발아전에 벼(Oryza sativa)에는 아무런 살초효과가 나타나지 않는 반면에 논피 (Echinochloa crus-galli)에만 살초효과가 보이는 선택성을 확인할 수 있었다. SAR분석 결과, 살초활성은 전자효과 (${\sigma}^*$)가 소수성 (logp)보다 2:1의 비율로 큰 영향을 미친다는 사실을 알았으며 이 같은 근거에 따라 alkoxy-기는 강한 전자밀게 (${\sigma}^*<0$)이고 소수성이 큰 (logp>0) alkyl기로 대체되어야 살초활성이 개선될 것으로 판단되었다.

• Bulletin of the Korean Chemical Society
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• 제16권11호
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• pp.1037-1042
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• 1995

The reaction of acetophenone 1-ureidoethylidenehydrazones 6 with a mixture of triphenylphosphine, carbon tetrachloride, and triethylamine in dichloromethane provides a general route to 1-(1-phenylethenyl)-5-(N-substituted amino)-1,2,4-triazoles 11 via the electrocyclization of the expected azino carbodiimide intermediates 9 to give the resonance stabilized azomethine imine 10a followed by a proton abstraction from the methyl group by amide anion. However, the same reaction of benzaldehyde 1-ureidoethylidenehydrazones 5 was unsuccessful. Under the same conditions, the reactions of benzaldehyde 1-N-acylureidoethylidenehydrazones 7 or acetophenone 1-N-acylureidoethylidenehydrazones 8 afforded 4H-1,2,4-triazolo[1,5-c][1,3,5]oxadiazines 16 or 17 via the zwitterionic species 15, or a [4+2] intramolecular cycloaddition from the carbodiimide intermediates 14, respectively.

• 약학회지
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• 제50권1호
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• pp.40-46
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• 2006

Square wave voltammetric (SWV) and cyclic voltammetric (CV) behaviors of cefotaxime sodium and ceftriaxone sodium have been investigated in the potential range between -0.10 V and -1.30 V using the phosphate buffers of various pH values ($2.00{\sim}9.10$). Two main peaks observed were irreversible and protons were involved in their electrochemical reductions. The first peaks of these cephalosporin antibiotics are due to the reduction of the azomethine double bond in the methoxyimino group of the side chain at position 7. The second peaks of cefotaxime sodium and ceftriaxone sodium are related to the reductions of the ${\Delta}^3$ double bond and the dioxo moiety of the side chain at position 3, respectively. The calibration curve of cefotaxime sodium in the concentration range between $1.0{\times}10^{-7}M$ and $1.0{\times}10^{-5}M$ yielded the linearity with the correlation coefficient of 0.9998 when the first peak of the antibiotic in a phosphate buffer of pH 3.02 was measured at the conditions of frequency of 120 Hz and pulse height of 50 mV by SWV. The present fast, simple and accurate SWV assay method was applied to determine cefotaxime sodium in the commercial antibiotic powder of injection.

• 농약과학회지
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• 제5권3호
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• pp.12-17
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• 2001

5-Benzofuryl-2-[1-(alkoxyimine) alkyl]-3-hydroxycyclohex-2-en-1-one 유도체중에서 2,3-dihydro-2,3,4,6,7-penta-methylbenzofuran-5-yl 그룹이 치완된 화합물(III)들의 벼(직파 및 3엽기)와 강피(Echinochloa crus-galli)에 대한 제초활성을 측정하고 alkoxy-치환체($OR_2$)가 변화함에 따른 구조와 제초활성과의 관계(SAR)를 정량적으로 검토한 결과, 직파벼와 강피 사이의 선택성 조건은 $R_1$=ethyl-이고 $R_2$-기는 비 대칭성의 적정값$(L/B_1)_{opt.}=3.96{\AA}$에 가까운 값을 갖는 치환체 이어야 할 것으로 판단되었다. 그리고 Free-Wilson 분석에 따르면 $R_2$-기는 $C_1{\sim}C_3$의 주로 불포화된 것들 중에서 특히, 3-chloro-2-propenyl기가 강피에 대한 제초활성을 가장 크게 나타내었다.

• 대한화학회지
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• 제30권5호
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• pp.441-448
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• 1986

몰리브덴산암모늄 수용액에서 적절한 살리실알데히드의 메탄올 혼합용액으로부터 디옥소비스(치환-살리실알데히다토) 몰리브덴늄(VI), $MoO_2(X-sal)_2(X=H,\;5-CH_3)$착물을 합성하고, 이들 각각의 화합물과 다양한 일차아민의 반응에 의하여 디옥소비스(치환-살리실알디미나토) 몰리브덴늄(VI)착물, $MoO_2(X-sal-N-R)_2,\;(R=C_6H_5,\;p-F-C_6H_4,\;m-Cl-C_6H_4,\;p-I-C_6H_4$ 및 $p-C_2H_5-C_6H_4)$을 합성하였다. 이들 착물은 모두 $900{\sim}940cm^{-1}$ 부근에서 ${\upsilon}_{Mo}=0$에 기인한 두 개의 강한 흡수띠가 관찰되었고, 핵자기공명스펙트럼에서 N=CH양성자에 대한 한 개의 시그날이 8.9ppm부근에서 나타났다. 이는 이들 착물이 $cis-MoO_2$기를 가진 6배위팔면체 착물임을 나타낸다. 질량분석의 결과로부터, $MoO_2$ : ligand의 결합비가 1:2임을 확인하였고, $MoO_2(5-CH_3-sal-N-R)_2$착물에 대한 분해과정을 조사하였다. 전자흡수스펙트럼에서 $N{\to}Mo$와 $O{\to}Mo$에 해당하는 전하이동전이는 $29,000cm^{-1}$과 $32,000cm^[-1}$부근에서 각각 일어났다. 한편, 디메틸포름아미드에서 측정한 이들 착물에 대한 몰전도도로부터 이들 착물이 비이온성 물질임을 확인하였다.

• 대한화학회지
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• 제65권2호
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• pp.93-105
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• 2021

Mononuclear Cu(II), Ni(II), Co(II), Mn(II), Zn(II), Fe(III), Ru(III), and UO2(II) complexes of 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide (H2L) were prepared by direct method. The ligand and its complexes were isolated in solid state and characterized by analytical techniques such as elemental and thermal analyses, molar conductance, magnetic susceptibility measurements and spectroscopic techniques such as UV-Visible, IR, 1H-NMR and 13C-NMR. The spectral data indicated that the ligand acted as neutral/monobasic bidentate or monobasic/dibasic tridentate ligand bonded to the metal ions through the oxygen atom of ketonic or enolic carbonyl group, azomethine nitrogen atom and deprotonated/protonated phenolic oxygen atom forming either tetragonally distorted octahedral or octahedral. Antimicrobial activities of the ligand and its complexes were evaluated against Escherichia coli, Bacillus subtilis and Aspergillus niger by well diffusion method. The results of antifungal activity showed that the Fe(III) complex (10) exhibited higher antifungal against Aspergillus niger than the other complexes. However, the results of antibacterial activity revealed that Cu(II) complex (4) is the most active against Escherichia coli while the Cu(II) complex (5) and Fe(III) complex (10) exhibited higher antibacterial effect on Bacillus subtilis than the other complexes.