• Title/Summary/Keyword: Liquid-phase synthesis

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Synthesis and Characterization of New Liquid Crystalline Fumarate and Maleate Monomers with Two Symmetrical Mesogens

  • 한양규;김경민
    • Bulletin of the Korean Chemical Society
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    • v.20 no.12
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    • pp.1421-1427
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    • 1999
  • 4-Hydroxy-4'-methoxyazobenzene and 4-hydroxy-4'-cyanoazobenzene were synthesized from phenol with p-anisidine and p-aminobenzonitrile through a diazotization reaction, respectively. They were reacted with 2-chloroethanol, 2-(2-chloroethoxy)ethanol, or 2-[2-(2-chloroethoxy)ethoxy]ethanol to produce six kinds of new mesogenic alcohols having an azobenzene group that is sensitive to the ultraviolet. Twelve kinds of new photoresponsive monomers with two symmetrical mesogens were prepared by the reaction of the mesogenic alcohols with fumaric acid or maleic acid through a Mitsunobu reaction. The resulting monomers have different length of flexible ethyleneoxy spacer tethered to azobenzene group. The length of the spacer affected their thermal stability, solubility, and phase transition temperature. Structures of the monomers were identified by FT-IR and ¹H-NMR spectra. Their phase transition temperatures and thermal stability were also investigated by a differential scanning calorimetry (DSC) and a thermogravimetric analysis (TGA). From an optical polarizing microscopy, all the prepared monomers except fumarate-1 and maleate-1 were found to show enantiotropic liquid crystallinity with a smectic texture like focal-conic, fan-shaped, and batonnet textures.

Liquid Crystalline Properties of Dimers Having o-, m- and p- Positional Molecular Structures

  • Park, Joo-Hoon;Choi, Ok-Byung;Lee, Hwan-Myung;Lee, Jin-Young;Kim, Sung-Jo;Cha, Eun-Hee;Kim, Dong-Hyun;Ramaraj, B.;So, Bong-Keun;Kim, Kyung-Hwan;Lee, Soo-Min;Yoon, Kuk-Ro
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1647-1652
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    • 2012
  • With the objective to design and synthesis of Schiff's base symmetrical liquid crystal dimmers and to study the effect of molecular structure variation ($o-ortho$, $m-meta$, $p-para$) and change in alkoxy terminal chain length on mesomorphic properties of liquid crystals, We have synthesized Schiff base dimers from dialdehyde derivative containing 2-hydroxy-1,3-dioxypropylene as short spacer with aniline derivatives having different lengths of terminal alkoxy chains ($n$ = 5, 7, 9). The chemical structure of the final products was characterized by proton nuclear magnetic resonance ($^1H$ NMR) spectroscopy and fourier transform infrared (FT-IR) spectroscopy. The mesomorphic properties and optical textures of the resultant dimers were characterized by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). The existence of smectic A phase transition was confirmed by the observation of batonnets and fan shaped textures in optical microscopy when compound were heated from crystalline phase. All of the dimers of this series, with the exception of $\mathbf{2S_5}$ -ortho, -meta, -para, were thermotropic liquid crystal. The compound $\mathbf{2S_9}$ -meta was monotropic, while the rest were enantiotropic. It was found that the change in terminal alkoxy chain length has pronounced effect on the mesomorphic properties. The temperature range of smectic A phase window widens with increasing alkoxy chain length.

Synthesis of Periodic Mesoporous Organosilica by Microwave Heating

  • Yoon, Sang-Soon;Son, Won-Jin;Biswas, Kalidas;Ahn, Wha-Seung
    • Bulletin of the Korean Chemical Society
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    • v.29 no.3
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    • pp.609-614
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    • 2008
  • A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.

An Efficient One-Pot Strategies for the Synthesis of [1,3] Oxazine Derivatives ([1,3] Oxazine 유도체 합성을 위한 효율적인 One-Pot 합성)

  • Sapkal, Suryakant B.;Shelke, Kiran F.;Shingate, Bapurao B.;Shingare, Murlidhar S.
    • Journal of the Korean Chemical Society
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    • v.54 no.4
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    • pp.437-442
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    • 2010
  • Sodium hydrogen sulphate ($NaHSO_4$), n-tetra butyl ammonium bromide (TBAB) as a phase transfer catalyst (PTC) in water, and 1-butyl-3-methyl imidazolium hydrogen sulphate [bmim]$HSO_4$ as ionic liquid (IL) has been used as a mild reaction promoter for the cyclocondensation of formalin, ${\beta}$-naphthol and aromatic amines to afford respective 2,3-dihydro-2-phenyl-1H-naphtho-[1,2-e] [1,3] oxazine derivatives. The present protocols are greener, high yielding and involved the nonchromatographic isolation procedure.

Aqueous synthesis of quantum dots using functionalized ionic liquid (이온성 액체를 이용한 수계 양자 점 합성)

  • Choi, Suk-Young;Kim, Tae-Young;Suh, Kwang-S.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.254-254
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    • 2010
  • We report aqueous synthesis of cadmium telluride (CdTe) quantum dots(QDs) using imidazolium-based ionic liquids with various functional groups. The functinalized ionic liquids were designed to have thiol groups, and then phase transfer with aqueous or organic solvents can be adjusted by changing side chain lengths of the cation and the choice of anion. The quantum yield was obtained IL-functionalized CdTe QDs reached up to 40% by post-treatment method.

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Synthesis of Ferroelectric Liquid Crystals Obtained from Optically Active l-isoleusine (광학활성 이소로이신을 출발물질로 한 강유전성 액정물질의 합성)

  • Jeong, N.H.;Kikuchi, H.;Kajiyama, T.
    • Journal of the Korean Applied Science and Technology
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    • v.13 no.3
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    • pp.51-60
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    • 1996
  • A new one series of chiral schiff's base containing benzylidene aniline moieties was synthesized and characterized by IR, $^1H$ NMR. elementary analysis, and polarized optical microscopy(POM). The yield of these synthetic compounds was in the range of $62{\sim}67^{\circ}C$. The results showed that most of the synthetic compounds were monotropic liquid crystal and exhibited chiral smectic C($Sc^{\ast}$) liquid crystal phases, and the range of phase transition temperature was to $71.4^{\circ}C$ from $45.0^{\circ}C$.

Synthesis and Mesomorphic Properties of Achiral Liquid Crystals with 1,3-Dialkoxy-2-propyl Swallow-Tail

  • Lee, Seng-Kue;Bang, Mi-Yeon;Lee, Jong-Gun;Kang, Kyung-Tae;Kim, Yong-Bae
    • 한국정보디스플레이학회:학술대회논문집
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    • 2003.07a
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    • pp.575-577
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    • 2003
  • Achiral swallow-tailed liquid crystals derived from 1,3-dialkoxy-2-propanol were prepared and their mesomorphic properties were investigated. 1,3-Dialkoxy-2-propyl swallow-tailed material showed antiferroelectric-like smectic C phase at lower temperature and in broader temperature range than the corresponding compounds with a branched alkyl group as a swallow-tail. They could serve as suitable host for antiferroelectric mixtures.

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Synthesis and Properties of Non-chiral Liquid Crystalline Molecules with Semi-Fluorinated Alkyl Chains

  • Choi, E-Joon;Sim, Hoo-Sik;Zin, Wang-Cheol;Kim, Dae-Cheol;Lee, Chong-Kwang;Chien, Liang-Chy
    • 한국정보디스플레이학회:학술대회논문집
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    • 2002.08a
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    • pp.933-935
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    • 2002
  • In this paper, new non-chiral molecules with semi-fluorinated alkyl chains were synthesized varying the structure of central bent core unit. Their mesomorphic properties were investigated by DSC and polarized microscopy. The compound with 1,3-dihydroxy phenylene unit could form an enantiomeric smectic phase, but the remaining compounds with bent-core mesogenic unit were not liquid crystalline. In this presentation, their x-ray measurement and electro-optical property will be also described.

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Synthesis and Properties of Thermotropic Compounds with Two Terminal Mesogenic Units and a Central Spacer Ⅲ. Homologous Series of $\alpha,\omega$-Bis[4-(p-nitrobenzoyloxy)phenoxy]alkanes

  • Jin, Jung-Il;Kang, Joo-Sam;Jo, Byung-Wook;Lenz, Robert W.
    • Bulletin of the Korean Chemical Society
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    • v.4 no.4
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    • pp.176-180
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    • 1983
  • A series of new liquid crystalline compounds having two identical mesogenic terminal units, the 4-(p-nitrobenzoyloxy)phenoxy group, attached to both ends of a central polymethylene spacer of various lengths was prepared. The mesomorphic properties of the compounds were investigated by differential scanning calorimetry (DSC) and by polarizing microscopy. Almost all of the compounds formed monotropic nematic mesophases. The trimethylene spacer compound was found to be non-liquid crystalline, while the one with the hexamethylene central spacer was enantiotropic. A thermodynamic analysis was performed for the phase transitions of the compounds and the results are discussed in relation to their liquid crystal properties.

Synthesis of BiSrCaCu(Ni)O Ceramics from the Gel Precursors and the Effect of Ni Substitution

  • Ahn, Beom-Shu
    • Bulletin of the Korean Chemical Society
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    • v.23 no.9
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    • pp.1304-1323
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    • 2002
  • Superconducting BiSrCaCu(Ni)O ceramicss have been prepared by the gel method using an aqueous solution containing a tartaric acid. The aqueous solution of metal salts was concentrated without precipitation. The precursor so prepared was homogeneou s and calcined at $825^{\circ}C$ for 24 h to produce superconducting phase. The thermal decomposition of gels, the formation of superconducting phase, and their ceramic microstructure were studied using IR, TGA, XRD, resistance measurements, and SEM. This method is highly reproducible and leads to powders with excellent homogeneity and small particle size for easy sinterability. The nickel dopant substituting for Cu gives rise to the gradual decrease of the Tc. Phase pure 2212 ceramics were obtained at 825 $^{\circ}C$ for 24 h. SEM pictures showed that liquid phase was formed when the samples were sintered temperatures higher than 825 $^{\circ}C$.