• Elastomers and Composites
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• 제26권4호
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• pp.296-303
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• 1991

Surface of crystalline silica was sequentially reacted with silane(A 187), liquid $rubber(CTBN{\times}8)$, and vinyl monomer(GMA) in existence of TEA(triethylamine) or BPO(benzoyl peroxide). It was mixed with epoxy resin at a ratio $0{\times}60%$ (vol. % ) of total component. For mixtures, viscous properties were investigated experimentally. 1) Coating ratio depended on pH of mixture and quantity of catalyst. 2) Treated silica represented lower viscosity than untreated. 3) Thixotropic index represented best at silica_content $15{\sim}23%$ and showed more large deviation over $120^{\circ}C$. 4) Relative viscosity followed kernel's at $0{\times}10%$ of silica content and get out of Mooney's at more than 15%.

• 약학회지
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• 제27권3호
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• pp.229-234
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• 1983

In the manufacture of precipitated sulfur calcium pentasulfide ($CaS_{5}$, train product) and calcium thiosulfate ($CaS_{2}O_{3}$, by-product) are decomposed simultaneously by hydrochloricacid into coarse (not being uniform) particle-size products. To improve this drawback, calcium thiosulfate was prepared directly without making calcium pentasulfide and obtained $S_{6}$ by the acid-decomposition. In the conversion of hexatomic sulfur to octatomic sulfur, the polymerization and the depolymerization were observed by using purification method. The conversion of $S_{6}$ to $S_{8}$ is proceeded by two steps. The first step reaction is affected by impurities (especially $SO_{2}$ and $H_{2}S$), Hexatomic sulfur is inert to triethylamine for the time being by purification, and thereafter a slow conversion to polymeric and then to octatomic sulfur occurs. Instead of calcium pentasulfide, the acid decomposition of calcium thiosulfate has several advantages; uniformity of particle-size of product, increase of yield, and simplicity of procedure.

• 약학회지
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• 제55권2호
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• pp.127-130
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• 2011

We synthesized new ${\alpha}$-amidoketenes using dehydrochlorination from anilines, triethylamine and malonyl dichloride under $0^{\circ}C$. The utility of ketenes in both laboratory and industrial practice was quickly recognized, and these species have been extensively utilized, including as pharmaceutical intermediates and anti-cancer agents. All synthetic process from anilines to ${\alpha}$-amidoketenes could be carried out by one-pot reaction. Synthetic ketenes 2a~f were identified using NMR and IR spectrum. Formation of ketenes was undertaken with dropping of malonyl dichloride at $0^{\circ}C$ in methylene chloride for 0.5~4 h. Using malonyl dichloride was better than using diethyl malonate as a synthetic reagents for the ketenes.

• Bulletin of the Korean Chemical Society
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• 제31권1호
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• pp.69-74
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• 2010

The new idarubicin analogues (12 and 13) with a glucose or galactoseas as a glycone were synthesized from daunomycin (2). (+)-4-Demethoxydaunomycinone (6) obtained from reaction of 2 with $AlCl_3$ was converted to 4-trifluoromethanesulfonyl daunomycinone (7) through reaction with trifluoromethanesulfonic anhydride. The treatment of 7 with 1,1-bis-(diphenylphospino)ferrocene/$Pd(OAc)_2$ in triethylamine/formic acid/dioxane provided the idarubicinone (5b). Glycosylation of 7-hydroxy group of 5b with two kinds of tetraacetyl pyranosyl halide (8 and 9) by a modified Koenigs-Knorr procedure and then deacetylation using aqueous 0.1 N LiOH solution and amberlite cationic resin gave the objective materials. The in vitro MTT assay of the analogues (12b and 13a) in comparison with idarubicin (5a) on peripheral blood human promyelocytic-leukemia cell line and human breast cancer cell line were also described.

• Environmental Analysis Health and Toxicology
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• 제12권3_4호
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• pp.1-13
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• 1997

First- and second-order kinetic oxidation rates of trichlorobenzenes (TCBs) were obtained and compared by a chemical activation system (CAS) which mimics mixed functional oxidase activity. The system consists of EDTA, ferrous sulfate, ascorbic acid, and $H_2O_2$ in potassium phosphdte buffer (monobasic at pH 7.4). The rate of transformation in CAS was enhanced in the presence and absence of catalase in the sequence 1, 2, 3-TCB < 1, 2, 4-TCB < 1, 3, 5-TCB. In general, the rates of degradation were greater in the test media with catalase. The effect of photolysis on the degradation of the TCBs with the CAS were examined. Sensitized photolysis with nitrite, Fenton's reagent, TiO$_2$ and triethylamine (TEA) studied in concert with the CAS demonstrated significant enhancement of the degradation rate of TCBs. Disappearance rates of TCBs in CAS with prior photolysis or prior photosensitization were at least 10-fold higher than the sum of the rate for each single experiment. This study proves that the combination of the CAS and photolysis can be used as a suitable technique for enhancing degradation of TCBs in aqueous systems.

• 약학회지
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• 제39권3호
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• pp.283-288
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• 1995

Rapid gas chromatographic profiling method was applied to saliva from healthy subjects for the analysis of free organic acids. Saliva samples were first saturated with NaHCO$_{3}$ and extracted with diethyl ether. The aqueous phase was solid-phase extracted using Chromosorb P as the adsorbent and diethyl ether as the eluent after the acidification and NaCl saturation, followed by triethylamine treatment. The resulting tiiethylammonium salts of acids were directly converted into stable tert.-butyl-dimethylsflyl derivatives, with subsequent analysis by dual-capiuary column gas chromatography and gas chromatograpy -mass spectrometry. From the ten saliva samples studied, twenty eight free organic acids including various fatty acids, hydroxy acids, dicarboxylic acids, md aromatic acids were tentatively identified. Among the acids identified , the concentration of lactic acid was highest for five saliva samples while $\alpha$-hydroxyisocaproic acid was most abundant for me sample, and succinic acid and glycolic acid for two samples. respectively. When the GC profiles were simplified to the corresponding acid retention index spectra of bar graphical form, they presented characteristic patterns for each individual.

• Bulletin of the Korean Chemical Society
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• 제24권12호
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• pp.1809-1813
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• 2003

Monomeric antioxidant 1 was prepared by the reaction of 3,5-di-tert-butyl-4-hydroxybenzyl alcohol with N-[4-(chlorocarbonyl)phenyl]maleimide in the presence of imidazole. Monomeric antioxidant 2, bearing carbamate group, was synthesized from the reaction of 3,5-di-tert-butyl-4-hydroxybenzyl alcohol and azidomaleimide. Antioxidant 3 was prepared by the reaction of N-(4-hydroxyphenyl)maleimide and 3-(3,5-ditert-butyl-4-hydroxyphenyl) propionic chloride in the presence of triethylamine. These reactive antioxidants were grafted onto polypropylene (PP) by melt-processing with free radical initiators in a mini-max moulder. From the infrared spectra of the grafted PP, it was found that the monomeric antioxidants were grafted onto PP. IR spectroscopic methods were used for the quantitative determination of the extent of grafting of monomeric antioxidant. To optimize the reaction conditions, the influences of the concentration of DCP, monomeric antioxidant, reaction time and temperature on the extent of grafting were studied.

• 대한화학회지
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• 제55권6호
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• pp.952-959
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• 2011

Novel phosphorylated derivatives of ribavirin 5-16 were synthesized by the reaction of 4-nitrophenyl phosphorodichloridate with various amino acid esters in the presence of triethylamine in dry tetrahydrofuran through the intermediates 3. On further reaction of 3 with ribavirin in THF and pyridine in the presence of TEA afforded the title compounds 5-16. Their structures were characterized by IR, $^1H$, $^{13}C$, $^{31}P$ NMR and mass spectral analyses. All the title compounds were found to exhibit potent in vitro anticancer activity against MCF-7 breast cancer cell lines.

• Bulletin of the Korean Chemical Society
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• 제28권5호
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• pp.751-757
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• 2007

To develop new COX-2 inhibitors, 1,5-diarylhydantoins and 1,5-diaryl-2-thiohydantoins were synthesized from phenylacetic acids by esterification, bromination, C-N bond formation and cyclization. Esters 1-3 were efficiently synthesized from the starting materials by reflux in absolute methanol for 3 h containing concentrated sulfuric acid as catalyst. Bromination was carried out with N-bromosuccinimide at rt in dichloromethane. Bromides 4-6 were reacted with aniline, p-anisidine, sulfanilamide in ethanol (or N,N-dimethylformamide) to provide the amines 7-15. Hydantoins and 2-thiohydantoins 16-46 were synthesized from amines 7-15 by treating them with potassium isocyanate (or potassium thiocyanate) and triethylamine. The synthetic process from alkyl α-anilinophenylacetate 7-15 to 3-alkylhydantoins was carried out in a one-pot reaction using alkyl isocyanate (alkyl isothiocyanate).

• 대한화학회지
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• 제62권3호
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• pp.187-190
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• 2018

A three-component coupling reaction of phenylacetylene, p-toluenesulfonyl azide, and water through copper catalysis is described to provide knowledge of spectroscopy and catalytic reactions and to introduce current research topics in organic chemistry for second-year undergraduate students. In the presence of stoichiometric amounts of phenylacetylene, p-toluenesulfonyl azide, and triethylamine, the reaction was performed with 4 mol% CuCl in water as the sole solvent and was completed in 1.5 h. A practical purification method and recrystallization of the crude reaction mixture resulted in the rapid isolation of the desired product with yields of 42~65%. Students characterized 4-methyl-N-(phenylacetyl)benzenesulfonamide by using melting-point determination, infrared spectroscopy, and nuclear magnetic resonance (NMR) spectroscopy. This experimental procedure and spectroscopic data analysis will serve as a platform for students to apply classroom knowledge in practical state-of-the-art research.