• Title/Summary/Keyword: Solid phase synthesis

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Direct Solid State Synthesis of Zn4Sb3 by Hot Pressing and Thermoelectric Properties (열간 압축 공정에 의한 Zn4Sb3의 직접 고상 반응 합성 및 열전특성)

  • Ur Soon-Chul
    • Journal of Powder Materials
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    • v.12 no.4 s.51
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    • pp.255-260
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    • 2005
  • Direct solid state synthesis by hot pressing has been applied in order to produce high efficiency $Zn_4Sb_3$ bulk specimens. Single phase $Zn_4Sb_3$ with 98.5% of theoretical density was successfully produced by direct hot pressing of elemental powders containing 1.2 at.% excess Zn. Thermoelectric properties as a function of temperature were investigated from room temperature to 600 K and compared with results of other studies. Transport properties at room temperature were also evaluated. Thermoelectric properties of single phase $Zn_4Sb_3$ materials produced by direct synthesis were measured and are comparable to the published data. Direct solid state synthesis by hot pressing provides a promising processing route in this material.

Solid-phase Synthesis of 7-Aryl-benzo[b][1,4]oxazin-3(4H)-one Derivatives on a BOMBA Resin Utilizing the Smiles Rearrangement

  • Lee, Ji-Min;Yu, Eun-Ae;Park, Joo-Yeon;Ryu, In-Ae;Shin, Dong-Soo;Gong, Young-Dae
    • Bulletin of the Korean Chemical Society
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    • v.30 no.6
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    • pp.1325-1330
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    • 2009
  • A general method has been developed for the solid phase synthesis of drug-like 7-aryl-benzo[b][1,4]oxazin-3(4H)- one derivatives 6. The method relies on a novel, microwave irradiation promoted cyclization reaction of the BOMBA resin bound, N-substituted-$\alpha$-(2-chloro-4-bromophenoxy)acetamide 3 that takes place via a Smiles rearrangement. The 7-bromobenzo[1,4]oxazine 4, produced in this process is converted to 7-aryloxazin analogs 5 by utilizing Suzuki coupling with various substituted arylboronic acids. Finally, the target 7-aryl-benzo[b][1,4]oxazin-3(4H)-ones 6 are liberated from the resin by treatment with 5% TFA. The progress of the reactions involved in this preparative route can be monitored by using ATR-FTIR spectroscopy on a single bead. The target compounds, obtained by using this five-step sequence, are produced in high yields and purities.

Simple and Highly Efficient Synthesis of [$^{11}C$]methionine Using Solid-Phase Extraction Method (고정상 추출법을 이용한 효율적인 [$^{11}C$]methionine의 합성)

  • Lim, Sung-Jae;Moon, Woo-Yeon;Choi, Jae-Chil;Cho, Shee-Man;Oh, Seung-Jun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.12 no.3
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    • pp.181-183
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    • 2008
  • We developed simple and highly efficient synthesis method for [$^{11}C$]methionine using solid-phase extraction method. For synthesis, we used C18 cartridge. [$^{11}C$]methionine was synthesized on C18 cartridge according to the solid-phase [$^{11}C$]methylation of precursor L-homocysteine thiolactone hydrochloride. The radiochemical yields of [$^{11}C$]methionine was $48.9{\pm}7.93%$ decay corrected (results of 30 syntheses, mean$\pm$SD), with average production higher than 180 mCi. This procedure showed high yield and simple synthesis of [$^{11}C$]methionine.

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Synthesis of Silicon Tracelsss Linker for Solid-Phase Reaction

  • Mun Han-Seo;Seong Jin-Hyun
    • Archives of Pharmacal Research
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    • v.27 no.4
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    • pp.371-375
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    • 2004
  • The silicon linker is the foremost traceless linker used in solid-phase reactions. Hydrogen fluo-ride (HF) or trifluoroacetic aicd (TFA) can remove the silicon linker with the silicon atom being replaced by a hydrogen atom. In this experiment, the linkers 1c and 2d, which are the most useful in solid-phase reactions, were synthesized, Linker 1c is composed of seven linearly linked carbons and linker 2d includes an oxygen atom in the linear carbon chain to increase the solvation capacity. The carboxylic acid component of linker 1c and 2d forms an amide or ester bond with resin. The synthesized linkers 1c and 2d could be utilized in constructing a chemical compound library that includes indole, benzodiazepine and phenothiazine (aromatic ring compounds).

Synthesis of Au Nanowires Using S-L-S Mechanism (S-L-S 성장기구를 이용한 양질의 골드 나노선 합성)

  • No, Im-Jun;Kim, Sung-Hyun;Shin, Paik-Kyun;Cho, Jin-Woo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.11
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    • pp.922-925
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    • 2012
  • Single crystalline Au nanowires were successfully synthesized in a tube-type furnace. The Au nanowires were grown by vapor phase synthesis technique using solid-liquid-solid (SLS) mechanism on substrates of corning glass and Si wafer. Prior to Au nanowire synthesis, Au thin film served as both catalyst and source for Au nanowire was prepared by sputtering process. Average length of the grown Au nanowires was approximately 1 ${\mu}m$ on both the corning glass and Si wafer substrates, while the diameter and the density of which were dependent on the thickness of the Au thin film. To induce a super-saturated states for the Au particle catalyst and Au molecules during the Au nanowire synthesis, thickness of the Au catalyst thin film was fixed to 10 nm or 20 nm. Additionally, synthesis of the Au nanowires was carried out without introducing carrier gas in the tube furnace, and synthesis temperature was varied to investigate the temperature effect on the resulting Au nanowire characteristics.

Synthesis of Zn4Sb3 by Solid State Reaction and Hot Pressing, and Their Thermoeletric Properties (고상 합성과 진공 압축성형에 의한 Zn4Sb3의 제조 및 열전특성)

  • Ur Soon-Chul
    • Korean Journal of Materials Research
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    • v.15 no.7
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    • pp.473-479
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    • 2005
  • Thermoelectric $Zn_4Sb_3$ alloys were synthesized by a conventional powder metallurgy process consisting of solid state reaction and hot pressing. Single phase $Zn_4Sb_3$ was successfully produced by the annealing of cold compact starting with the mixed elemental powders, and subsequent hot pressing yielded single phase bulk specimens without microcracks. Phase transformations in this alloy system during synthesis were investigated using XRD, SEM and EDS. Thermoelectric properties as a function of temperature were investigated from room temperature to 600 K and compared with results of analogue studies. Transport properties at room temperature were also evaluated. Thermoelectric properties of single phase $Zn_4Sb_3$ materials produced by this process are comparable to the published data. Synthesis by solid state reaction and hot pressing offers a potential processing route to produce a bulk $Zn_4Sb_3$