• Journal of the Korean Chemical Society
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• v.65 no.2
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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.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.311-318
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• 2016

Azorubine is a synthetic tar color containing azo-bond in the molecular structure. This food colorant has been allowed to be used for beverages, cheese and dried fruits in the European Union and for some food in Australia. Even though it is applicable as a food color in many countries, this compound has not been permitted in Korea so far as a food additive. Thus, this study was performed to establish an analysis method for azorubine in Korea by comparison of three HPLC analysis methods for azorubine and other azo-compounds which are officially used in the European Food Safety Authority (EFSA, EU), the Food Standard Agency (FSA, England) and the National Institute of Food and Drug Safety Evaluation (NIFDS, Korea). The analysis method of the FSA for azorubine showed the best linearity ($r^2=0.999$), limit of detection (LOD, $0.07{\mu}g/mL$), limit of quantification (LOQ, $0.20{\mu}g/mL$), precision (0~0.5%) and accuracy (98.6~100.7%) among tested HPLC methods using a C-18 column and diode array detector (DAD) with ammonium acetate solution and acetonitrile as an eluent solution. Finally selected method of FSA was further verified by inter-day and intra-day experiments with linearity, LOD, LOQ, precision and accuracy. Recovery test showed the recover ratios of 97~103%, 95~101%, and 93~102% in beverages, breads/snacks and other foods, respectively. Inter-laboratory test represented the absolute value of z-score of less than 2 which means satisfactory levels in this test. Selected method of FSA showed reliable analytical results in application test using food samples collected in commercial markets in Europe.

• YAKHAK HOEJI
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• v.19 no.2
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• pp.101-110
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• 1975

p-Chloronitrobenzene(substrate) and p-nitrophenetole (product) were quantitatively analyzed to know the degree of extent of reaction in the process of time. The calibration curve was prepared by the internal satndard method in gaschromatography. 2,6-Dimethyl-naphthalene was used as internal standard. The rate constant(k), the reaction velocity in various concentrations of NaOH altered, and the formation of byproducts(azo-compound and p-nitrophenol) with the amounts of MnO$_{2}$ and NaOH altered, were studied. From the results of these of MnO$_{2}$ and NaOH altered, were studied. From the results of these experiments, this reaction was second order and the rate constant was k=10.3 $\times$ 10$^{-3}$ mole$^{-21$. When p-chloronitrobenaene 1 pt. NaOH 0.56pts. MnO$_{2}$ 0.5pts. and ethanol 25 pts-were reacted about 10 hours, p-nitrophenetole was nearly quantitatively obtained without byproducts.

• Polymer Science and Technology
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• v.3 no.4
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• pp.275-284
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• 1992

지금까지 우리는 환상 단량체들을 이용한 macroinitiators 및 이들을 이용한 block 고중합체들의 합성방법론에 대해 고찰해 보았다. 이 방법들 중 living polymerization은 block 공중합체의 합성 뿐 만아니라 macroinitiator와 같은 기능성화된 고분자 합성을 위한 최적의 방법이다. 여기서 우리가 지적하고 싶은 것은 macroinitiator라는 과학적인 의미의 혼돈이다. 특히 macroinitiator와 macromolecular initiator는 같은 scientific terms들로서 혼돈이 있어서는 안되며 macroazoinitiator 역시 azo group을 가진 macromolecular initiator의 한 종류이다. 또한 macroinitiator와 macromonomer를 혼돈해서는 안되며 macroinitiator는 block 그리고 macromonomer는 graft 공중합체 및 Network 고분자 제조에 각각 이용되는 기능성화된 고분자(functionalized polymer) 혹은 oligomer를 의미한다.

• Bulletin of the Korean Chemical Society
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• v.34 no.7
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• pp.2086-2092
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• 2013

Two new high-nitrogen energetic compounds $ZTO{\cdot}2H_2O$ and $ZTO(phen){\cdot}H_2O$ have been synthesized (where ZTO = 4,4-azo-1,2,4-triazol-5-one and phen = 1,10-phenanthroline). The crystal structure, elemental analysis and IR spectroscopy are presented. Compound 1 $ZTO{\cdot}2H_2O$ crystallizes in the orthorhombic crystal system with space group Pnna and compound 2 $ZTO(phen){\cdot}H_2O$ in the triclinic crystal system with space group P-1. In $ZTO(phen){\cdot}H_2O$, there is intermolecular hydrogen bonds between the -NH group of ZTO molecule (as donor) and N atom of phen molecule (as acceptor). Thermal decomposition process is studied by applying the differential scanning calorimetry (DSC) and thermo thermogravimetric differential analysis (TG-DTG). The DSC curve shows that there is one exothermic peak in $ZTO{\cdot}2H_2O$ and $ZTO(phen){\cdot}H_2O$, respectively. The critical temperature of thermal explosion ($T_b$) for $ZTO{\cdot}2H_2O$ and $ZTO(phen){\cdot}H_2O$ is $282.21^{\circ}C$ and $195.94^{\circ}C$, respectively.

• Proceedings of the KIEE Conference
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• 1999.07d
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• pp.1971-1973
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• 1999

Monolayers of azo-benzene group containing fatty acids(8A5H) were made by spreading and compressing on the water surface. These monolayers were optically stimulated by illuminating the lights of 365[nm] and 450[nm] from X-non lamp, and the structural changes of the molecules were measured by the displacement current method. Also, the dynamic behaviors of these monolayers were measured by the $\pi-A$ isotherms when changing the temperatures of the water surface. As results, when the monolayers were stimulated by 365[nm] light, the positive currents which were generated by the structural changes from trans to cis were measured. But the negative currents of the structural changes from cis to trans were too weak to detect. When the temperatures of the water surface were increased, surface pressures of the monolayers increased early because of the thermal activations of the molecules, and the double liquid film phase were disappeared upon $40[^{\circ}C]$.

• Journal of the Korean Chemical Society
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• v.23 no.6
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• pp.412-416
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• 1979

Although isotactic polypropylene gives an excellent fiber having high tenacity, abrasion resistance and chemical stability, it has not been widely used as a fabric for chlothing because of its poor dyeability. A number of methods for improvement of its dyeability have been proposed, but they were too complicated and/or gave damage its original excellent properties of polypropylene. We now wish to report the synthesis of a new reactive dye for polypropylene fiber by means of carbenic process. A reactive dye was synthesized from azo disperse dye having an aldehyde group and tosylhydrazine. By using this synthesized reactive dye, polypropylene fiber was dyed to thick and fast color.

• Journal of the Korean Chemical Society
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• v.28 no.6
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• pp.425-432
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• 1984

We obtained fast dyed polypropylene fiber, which has no functional group to be dyed, by producing a carbene on the dye molecule by the pyrolysis of lithium salt of dye molecule-tosylhydrazone, then the carbene simultaneously inserted into a C-H bond of polypropylene. To investigate the possibility of actual use in the industry, a variety of reactive azo dyes were prepared from aldehyde, acetophenone and benzophenone derivatives by changing reactive site of precursors which greatly affected properties of dyes. Reactive dyes of the benzophenone derivatives were excellent in the reaction with polypropylene, especially, a dye prepared from chloroaminobenzophenone with N,N-dimethyl aniline was found most excellent.

• Journal of the Korean Chemical Society
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• v.17 no.4
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• pp.275-285
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• 1973

The addition of one mole of aluminum chloride to three moles of sodium borohydride in tetrahydrofuran gives a turbid solution with enormously more powerful reducing properties than those of sodium borohydride itself. The reducing properties of this reagent were tested with 49 organic compounds which have representative functional groups. Alcohols liberated hydrogen immediately but showed no sign of hydrogenolysis of alkoxy group. Aldehydes and ketones were reduced rapidly within one hr. Acyl derivatives were reduced moderately, however, carboxylic acids were reduced much more slowly. Esters, lactones and epoxides were reduced readily than sodium borohydride or borane. Tertiary amide was reduced slowly, however, primary amide consumed one hydride for hydrogen evolution but reduction was sluggish. Aromatic nitrile was reduced much more readily than aliphatic nitrile. Nitro compounds were inert to this reagent but azo and azoxy groups were slowly attacked. Oxime was reduced slowly but isocyanate was only partially reduced. Disulfide and sulfoxide were attacked slowly but sulfide and sulfone were inert. Olefin was hydroborated rapidly.

• Bulletin of the Korean Chemical Society
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• v.15 no.2
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• pp.132-138
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• 1994

Bis(diethylamino)aluminum hydride was utilized in a systematic study of the approximate rates and stoichiometry of the reaction of excess reagent with 55 selected organic compounds containing representative functional groups under standardized conditions (THF, $0^{\circ}C$, reagent to compound=4 : 1) in order to define the characteristics of the reagent for selective reductions. The reducing action of BEAH was also compared with that of the parent aluminum hydride. The reducing action of the reagent is quite similar to that of aluminum hydride, but the reducing power is much weaker. Aldehydes and ketones were readily reduced in 1-3 h to the corresponding alcohols. However, unexpectedly, a ready involvement of the double bond in cinnamaldehyde was realized to afford hydrocinnamyl alcohol. The introduction of diethylamino group to the parent aluminum hydride appears not to be appreciably influential in stereoselectivity on the reduction of cyclic ketones. Both p-benzoquinone and anthraquinone utilized 2 equiv of hydride readily without evolution of hydrogen, proceeded cleanly to the 1,4-reduction products. Carboxylic acids and acid chlorides underwent reduction to alcohols slowly, whereas cyclic anhydrides utilized only 2 equiv of hydride slowly to the corresponding hydroxylacids. Especially, benzoic acid with a limiting amount of hydride was reduced to benzaldehyde in a yield of 80%. Esters and lactones were also readily reduced to alcohols. Epoxides examined all reacted slowly to give the ring-opened products. Primary and tertiary amides utilized 1 equiv of hydride fast and further hydride utilization was quite slow. The examination for possibility of achieving a partial reduction to aldehydes was also performed. Among them, benzamide and N,N-dimethylbenzamide gave ca, 90% yields of benzaldehyde. Both the nitriles examined were also slowly reduced to the amines. Unexpectedly, both aliphatic and aromatic nitro compounds proved to be relatively reactive to the reagent. On the other hand, azo- and azoxybenzenes were quite inert to BEAH. Cyclohexanone oxime liberated 1 equiv of hydrogen and utilized 1 equiv of hydride for reduction, corresponding to N-hydroxycyclohexylamine. Pyridine ring compounds were also slowly attacked. Disulfides were readily reduced with hydrogen evolution to the thiols, and dimethyl sulfoxide and diphenyl sulfone were also rapidly reduced to the sulfides.