• Bulletin of the Korean Chemical Society
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• v.12 no.4
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• pp.392-397
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• 1991

A stereocontrolled synthesis of (${\pm}$)-isocomene (1) via selective monoketalization of tricyclo[6.3.0.$0^{1.5}$]undeca-4,7-dione(13) was reported. Grignard reaction of bicyclic enone 10, which was prepared from 2-methyl-1,3-cyclopentadione, gave the 1,4-addition product 11. The subsequent aldol condensation product 12 was converted to mesyl derivative 13. Transformation from 13 to the desired product 19 was achieved by a series of reactions, i.e., the selective monoketalization at C-4 carbonyl group, the elimination of a mesyl group, Birch alkylation, methylation at C-6, the reduction of carbonyl group, the dehydration of alcohol 18, and hydrolysis of the ketal group.

• YAKHAK HOEJI
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• v.48 no.3
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• pp.202-206
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• 2004

New asymmetric dimers, N,N'-dialkyl-4'-hydroxy-4-oxo-2,2',3,3'-tetrahydro-2,2'-diphenyl-4,4'-quinolones 3a-f were synthesized through the dehydration and dea1coholation of N-alkylanilines and ethyl benzoylacetate. Dimers 3a-f were identified by NMR, IR and GC-MS. A series of dimer 3a-f has been synthesized using acid-catalyzed one-pot reaction that involved the condensation, cyc1ization and dimerization. Similarly, the 6,6'-methoxy (or 7,7'-methoxy) substituted dimers were prepared from N-alkyl-meta-(or para)-anisidines. Formation of dimers was undertaken with p-toluenesulfonic acid (p-TSA) at 90∼11$0^{\circ}C$ in toluene for 2∼6 hours over the Dean-Stark apparatus.

• Membrane Journal
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• v.7 no.2
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• pp.65-74
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• 1997

Pervaporation pilot tests for obtaining the anhydrous ethanol, which is an automobile fuel additive for reducing air pollution, were carried out in the production field of fermented ethanol by using a PVA composite membrane. In the pervaporation dehydration of the ethanol/water azeotropic mixture, the membrane performance is concluded to be enhanced with the heating temperature of feed. In the determination of the permeate condensation temperature from the viewpoint of energy cost, an Optimal temperature was found to be near $0{\circ}C$. The results on the dehydration of fermented ethanol were similar to those of synthetic ethanol, which indicates that the pervaporation performance is not influenced by impurities contained in the ethanol to be dehydrated. From a comparison of calculated energy needed in the system and measured value in the pilot test, it is confirmed that the latent heat for vaporization of permeant on the permeate side of membrane is supplied from the feed.

• Applied Chemistry for Engineering
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• v.21 no.4
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• pp.424-429
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• 2010

6-Alkyl-3-chromonealdehyde (2,2-dialkyl)hydrazone derivatives were synthesized by dehydration condensation. They are green-emitting materials for organic light emitting device (OLED) composed of electron acceptor of 6-alkyl-3-chromonealdehydes and electron donor of 2,2-dialkylhydrazones in a conjugated structure. The structural properties of reaction products were analyzed by FT-IR and $^1H$-NMR spectroscopy. The thermal stabilities and reactivities were measured by melting points and yields. The UV-visibles and PL properties were also determined by excitation spectra and emission spectra, respectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.04a
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• pp.155-159
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• 2003

The preparation and luminescence characterization of yttrium oxide doped with trivalent europium phosphors by sol-gel method have been investigated. Aqueous metal nitrate solution was mixed with EDTA which was chosen by the most suitable material of sol-gel formation one of appled various chelating agents. we noticed that the samples when are heated with EDTA at a temperature of $100^{\circ}C$ for 1hrs, produced brownish and crisp powders due to condensation reaction on decomposition, dehydration and formation of sol-gel. Hence, when the powder pre-heated was then heated at $1200^{\circ}C$ for 3hrs in atmosphere, the luminescence characterization of resultant $Y_{2}O_{3}:Eu^{3+}$ phosphor was enhanced upto maximum 30% significantly than conventional method through increasing porous region and decreasing particle sizes.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.04a
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• pp.151-154
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• 2003

The synthesis and luminescent properties of trivalent europium activated gadolinium oxide red phosphors by sol-gel process have been investigated. Aqueous metal nitrate solution was mixed with EDTA which was chosen by the most suitable material of sol-gel formation as chelating agents. We noticed that the samples when are heated with EDTA at a temperature of $100^{\circ}C$ for lhrs, produced brownish and crisp powders due to condensation reaction on decomposition, dehydration and formation of sol-gel. Hence, when the powder pre-heated at about $100^{\circ}C$ was then heated at $1200^{\circ}C$ for 3hrs in atmosphere, the luminescence properties of resultant $Gd_{2}O_{3}:Eu^{3+}$ phosphor was measured by SEM, FT-IT and brightness intensity was shown 20% higher than those prepared by conventional method and by other chelating agent.

• Applied Chemistry for Engineering
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• v.20 no.6
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• pp.670-674
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• 2009

3-Chromonealdehyde(2,2-disubstituted)hydrazone derivatives were synthesized by dehydration condensation. They are green-emitting materials for organic light emitting device (OLED) composed of electron acceptor of 3-chromonealdehydes and electron donor of 2,2-disubstituted hydrazones by a conjugated structure. The structural properties of reaction products were analyzed FT-IR and $^1H-NMR$ spectroscopy. The thermal stabilities and reactivities were measured by melting points and yields. The UV-visibles and PL properties can be determined by excitation spectra and emission spectra, respectively.

• Applied Chemistry for Engineering
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• v.20 no.1
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• pp.40-45
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• 2009

N-Alkylcarbazole-3-vinylene-2-methyl-4-dicyanomethylene-4H-pyran derivatives were synthesized by dehydration, $S_N2$, Vilsmeier, and Knoevenagel condensation. They are red-emitting materials for organic light emitting device (OLED) composed of electron donor of N-alkylcabazole-3-vinylene groups and electron acceptor of 2-methyl-4-dicyanomethylene-4H-pyran groups by a conjugated structure. The structural properties of reaction products were analyzed FT-IR and $^1H-NMR$ spectroscopy. The thermal stabilities and reactivities were measured by melting points and yields. The UV-visibles and PL properties can be determined by exitation spectra and emission spectra, respectively.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.02a
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• pp.264-264
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• 2012

As an environment-friendly alternative energy resource, ethanol may be used to obtain hydrogen, a clean energy source. Thus, studies on catalytic reactions involving ethanol have been studied to understand the underlying principles in the reaction mechanism using various oxide-supported catalysts. Among them, Au-based catalysts have shown a superior activity in producing hydrogen gas. In the present study, Au/$TiO_2$ catalysts were prepared by deposition-precipitation method to understand their catalytic activities toward ethanol and acetaldehyde with increasing gold loading, especially at the very low Au loading regime. A commercially available $TiO_2$ (Degussa P-25) was employed and the Au loading was varied to 0, 0.1, 0.5, and 1.0 wt% respectively. The catalysts showed characteristic x-ray diffraction (XRD) features at $2{\theta}=78.5^{\circ}$ that could be assigned to the presence of gold nanoparticles. Its reactivity measurements were performed under a constant flow of ethanol and acetaldehyde at a flow rate of ${\sim}0.6{\mu}mol/sec$ and the substrate temperature was slowly raised at a rate of 0.2 K/sec. We observed that the overall reactivity of the catalysts increased with increasing Au loading along with selectivity favoring dehydrogenation to product hydrogen gas. In addition, we disclosed various reaction channels involving competitive reaction paths such as dehydrogenation, dehydration, and condensation. In addition, subsequent reactions of acetaldehyde obtained from dehydrogenation of ethanol, were found to occur and produce butene, crotonaldehyde, furan, and benzene. Based on the results, we proposed overall reaction pathways of such reaction channels.

• Clean Technology
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• v.22 no.4
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• pp.250-257
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• 2016

As an attempt to replacing petroleum-based chemicals with bio-based ones, synthesis of furfural from biomass-derived xylose attracts much attention in recent days. Conventionally, furfural from xylose has been produced via the utilization of highly corrosive, toxic, and environmentally unfriendly mineral acids such as sulfuric acid or hydrochloric acid. In this study, microwave-assisted biphasic reaction process in the presence of novel bio-based heterogeneous acid catalysts was developed for the eco-benign and effective synthesis of furfural from xylose. The microwave was irradiated for reaction acceleration and a biphasic system consisting of $H_2O$ : MIBK (1 : 2) was designed for continuous extraction of furfural into the organic phase in order to reduce the undesired side products formed by decomposition/condensation/oligomerization in the acidic aqueous phase. Moreover, sulfonated amorphous carbonaceous materials were prepared from wood powder, the most abundant lignocellulosic biomass. The prepared catalysts were characterized by FT-IR, XPS, BET, elemental analysis and they were used as bio-based heterogeneous acid catalysts for the dehydration of xylose into furfural more effectively. For further optimization, the effect of temperature, reaction time, water/organic solvent ratio, and substrate/catalyst ratio on the xylose conversion and furfural yield were investigated and 100% conversion of xylose and 74% yield of furfural was achieved within 5 h at $180^{\circ}C$. The bio-based heterogeneous acid catalysts could be used three times without any significant loss of activity. This greener protocol provides highly selective conversion of xylose to furfural as well as facile isolation of product and bio-based heterogeneous acid catalysts can alternate the environmentally-burdened mineral acids.