• Journal of the Korean Chemical Society
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• v.55 no.4
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• pp.650-655
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• 2011

Three new peptide analogs 5a-c were obtained through coupling of 5-Amino benzimidazoles 2a-c with L-phenylalanine. For the purpose ${\alpha}$-amino group was blocked with phthalic anhydride and activation of ${\alpha}$-carboxy group of phenylalanine was carried out by preparing phthaloyl-L-phenylalanyl chloride 4. After developing a successful peptide linkage, the phthaloyl group was removed by treating 5a-c with hydrazine hydrate to get free peptides 6a-c, purified through a column of Amberlite (IR-4B). All of these compounds 2a-c and 5,6a-c have been characterized on the basis of their IR, 1H NMR and EIMS analyses. Antibacterial activity of these compounds is also been reported.

• Journal of the Korean Applied Science and Technology
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• v.29 no.3
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• pp.429-434
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• 2012

A kind of Antihistamines, Azelastine HCl which known as modern H1-blockers, was synthesized by four step process using phthalic anhydride, 4-chlorophenylacetic acid, hydrazine 2HCl. The first step was the reaction of removing carboxyl group and hydroxyl group and the second step was saponification of 3-(4-chlorobenzylidene)phthalide. The third step was the nucleophilic addition reactions of primary amines and the fourth step was addition reaction of N-methyl-1-aza-bicyclo[3,2,0]heptane to 4-(4-chlorobenzyl)-1-(2H)phthalazinone. As a result, product was analyzed by FT-IR and $^1H$-NMR and could be obtained with a yield of 80%.

• Journal of the Korean Society of Clothing and Textiles
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• v.29 no.12 s.148
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• pp.1608-1618
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• 2005

The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeration at $7^{\circ}C$ (LT), room temperature (RT), oven treatment at $100^{\circ}C$ (OV), and $H_2O_2/UV(PER)$ method. Degradation times for each thermal system were 6 hour, 24 hour, 48 hour, 1 week, 2 week, 4 week. Alizarin was detected from the control and degraded samples of both alizarin dyed and madder dyed fabrics. Benzoic acid, 2, 4-di-tert-butylphenol, phthalic anhydride were detected as the degradation products for both alizarin dyed and madder dyed fabrics. The result suggest that these products can be used as the fingerprints of GC-MS analysis for the identification of madder dye in archaeological textiles. Both alizarin dyed and madder dyed samples became less red and less yellow after degradation. In the PER degradation system madder dyed sample showed the greatest color difference even after 1 week of degradation treatment. Further research is necessary for investigating the color change in the exhumed textiles, which is caused by the dual action of dye fading and the staining of organic matters in the soil.

• Applied Chemistry for Engineering
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• v.4 no.4
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• pp.823-829
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• 1993

The basic medium oil modified alkyd resin was synthesized from linseed oil fatty acid(LOFA), phthalic anhydride(PAA), trimellitic anhydride(TMA ), and trimthylol propane(TMP) by condensation polymerization at $230^{\circ}C$. TMPTA modified water-reducible alkyd resins were synthesized with TMPTA graft copolymerization onto the basic resin at $180^{\circ}C$. Acid value of the resin was controlled by the addition of TMA and N,N-Dimethylethanol amino(DMEA) was used as an neutralizing agent to prepare water-reducible alkyd. To evaluate the optimum formulation for anionic alkyd resin, water proofness and water reducibility were estimated from the acid value or TMA contents. The effect of TMPTA on the graft copoymerization of the resin was studied by measuring molecular weight, glass transition temperature(Tg), viscosity, and gel contents. The suitable balance of water proofness and water reducibility of the resin was obtained at range of 5.3~7.0wt.% of TMA contents or 40~50 of acid value of basic resin. The molecular weight, viscosity, and gel contents of water-reducible alkyd resin were increased according to the TMPTA graft copolymerization, but Tg was decreased.

• Applied Chemistry for Engineering
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• v.5 no.4
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• pp.698-705
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• 1994

The basic medium oil modified alkyd resin was synthesized from linseed oil fatty acid(LOFA), phthalic anhydride(PAA), maleic anhydride(MA) and trimethylol propane(TMP) by condensation polymerization at $230^{\circ}C$. MA/TMPTA modified water-reducible alkyd resins were synthesized with TMPTA graft copolymerization onto the basic resin at $180^{\circ}C$. Acid value of the resin was controlled by the addition amount of MA and N,N-dimethylethanol amine(DMEA) was used as a neutralizing agent to prepare of the water-reducible alkyd resin. The effect of TMPTA on the graft copolymerization of the resin was studied by measuring molecular weight glass transition temperature(Tg), viscosity, graft efficiency, and gel contents of melanin cured film. Heat resistance, UV resistance and water resistance of cured film of MA/TMPTA modified resin was compared to those of TMA/TMPTA modified alkyd resin. The molecular weight, viscosity gel contents and graft efficiency of water reducible alkyd resin were increased according to the TMPTA graft copolymerization, but Tg was decreased. The viscosity was lower when the solid contents reached 40% than that of 30% content and also and also became lower with the extent of neutralization ratio, The heat resistance, UV resistance and water resistance of the MA/TMPTA modified alkyd resis were better than those of TMA/TMPTA modified alkyd resin but the storage stability of the TMA/TMPTA alkyd resis was better than that of MA/TMPTA modified alkyd resin.

• Fibers and Polymers
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• v.5 no.2
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• pp.83-88
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• 2004

In order to assess the potential of the hydroxy-containing polyamic acid (PHAA) synthesized from 3,3'-dihydroxy benzidine and pyromellitic dianhydride for a fire-safe polymer, the cyclization pathway of PHAA has been investigated using a model compound prepared from 2-aminophenol and phthalic anhydride. The reaction was monitored. by $^1{H-nuclear}$ magnetic resonance. N-(2-hydroxyphenyl) phthalamic acid is converted to N-(2-hydroxyphenyl) phthalimide at ca. 175$^{\circ}C$, showing endothermic reaction. The imide structure is rearranged to the benzoxazole structure over ca. $400^{\circ}C$. These results are similar with that of PHAA. According to pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) data, water and carbon dioxide are released during the cyclization and rearrangement reaction. One DMAc molecule is complexed with one carboxyl acid group in PHAA, which accelerates the imidization process to release more easily the flame retardant, water.

• Polymer(Korea)
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• v.38 no.6
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• pp.774-781
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• 2014

Acetylenic or phenylethynyl end-capped polyisoimide oligomers ($M_w$ 2500 g/mol, 5000 g/mol) based upon 4,4'-diamino diphenyl ether (4,4'-ODA)/4,4'-oxydiphthalic anhydride (ODPA) and 4,4'-ODA/3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BTDA) were synthesized by using 4-ethynylaniline (4-EA) or 4-phenylethynyl phthalic anhydride (4-PEPA) as an end capper. The incorporation of ethynyl groups were confirmed by FTIR spectroscopy. The isomerization temperature was influenced by molecular weight as well as the backbone structure of polyisoimides oligomers. Thus, polyisoimide oligomers with molecular weight of 2500 g/mol was found to be imidized at temperature $10^{\circ}C$ lower than that for the oligomers with molecular weight of 5000 g/mol. The crosslinking reaction of ethynyl groups occurred at a higher temperature than that for the isoimide/imide isomerization reaction. These two reactions were totally or partially overlapped on the DSC thermograms for the polyisoimide oligomer end-capped with 4-EA. Kinetics of thermal imidization and crosslinking reactions for the 4,4'-ODA/ODPA polyisoimide oligomers end-capped with 4-PEPA were investigated by performing dynamic DSC experiments at heating rate of $10^{\circ}C/min$. The activation energy and pre-exponential factors were 141 kJ/mol and $1.45{\times}10^{13}min^{-1}$ for the imidization reaction and 177 kJ/mol and $2.90{\times}10^{13}min^{-1}$ for the crosslinking reaction, respectively.

• Applied Chemistry for Engineering
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• v.8 no.4
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• pp.700-703
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• 1997

7-Aminocephalosporanic acid(7-ACA) was reacted with diphenyldiazomethane(DPM) to get diphenylmethyl 7-$\beta$-(O-ethylphthalimidomethylphosphony1)-3-acetoxymethyl-3-cephem-4-carboxylate. Diethyl phthalimidomethylphosphonate was chloridated with a slight excess of phosphorus pentachloride to the O-ethyl phthalimidoalkylphosphonochloridate. Previously unreported two compounds, diphenylmethy1 -7-$\beta$-(O-ethylphthalimidomethylphosphony1)-3-acetoxymethyl-3-cephem-4-carboxylate and diphenylmethyl-7-$\beta$-[O-ethylphthalimidoethylphosphonyl]-3-acetoxymethyl-3-cephem-4-carboxylate were synthesized by cupling reaction of DPM 7-ACA and O-ethyl phthalimidoalkylphosphonochloridate. All of the compounds including starting materials and reaction intermediates were characterized by $^1H$ NMR and FT-IR spectroscopy.

• YAKHAK HOEJI
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• v.35 no.5
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• pp.389-393
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• 1991

A convenient method for the synthesis of indobufen, which is a potent antiinflammatory agent, was described. Ethyl 2-phenylbutyrate(4) was prepared by Friedel-Crafts reaction of benzene with ethyl $\alpha$-chloro-$\alpha$-(methylthio)acetate(l) followed by ethylation and desulfurization of the resultant ethyl 2-(methylthio)phenylacetate(2). Ethyl 2-(p-aminophenyl)butyrate(6) was prepared by nitration of (4) and successive reduction of ethyl 2-(p-nitrophenyl) butyrate(5). Indobufen was obtained by condensation reaction of (6) with phthalic anhydride followed by reduction and hydrolysis of the resultant ethyl 2-[p-(1, 3-dioxo-2-isoindolinyl)phenyl]butyrate(7).

• Journal of the Korean Chemical Society
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• v.16 no.2
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• pp.84-92
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• 1972

A mechanism for the ring formation of nickel phthalocyanine (Ni-Pc) has been proposed based on chemical kinetics. The effect of the catalyst on the rate was examined, and ammonium molybdate has been found to be the most effective. The reaction order of the ring formation was determined to be of the 1st order over all, with only the concentration of urea affecting the rate of the ring formation. All the results including thermodynamic parameters support a conclusion that the rate-determining step seems to be the enolization of the urea-catalyst transition complex, followed by fast decomposition of the tautomeric enolized urea into ammonia and isocyanic acid. These intermediates then reacted with the phthalic anhydride to form imino and diimino-phthalimide, which condense to form nickel phthalocyanine in the presence of the nickel cation.