• Title/Summary/Keyword: Solvent Free Synthesis

검색결과 120건 처리시간 0.026초

Neat Synthesis and Anti-oxidant Activity of α-Hydroxyphosphonates

  • Rao, K. Uma Maheswara;Sundar, Ch. Syama;Prasad, S. Siva;Rani, C. Radha;Reddy, C. Suresh
    • Bulletin of the Korean Chemical Society
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    • 제32권9호
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    • pp.3343-3347
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    • 2011
  • A simple efficient and neat synthesis of ${\alpha}$-hydroxy phosphonates has been accomplished from aromatic/heterocyclic aldehydes and diethyl phosphite using $KHSO_4$ as a catalyst under solvent-free conditions at ambient temperature. These compounds are characterized by spectral and analytical data and tested for their anti-oxidant activity.

Selective Tandem Synthesis of Oximes from Benzylic Alcohols Catalyzed with 2, 3-Dichloro-5, 6-dicyanobenzoquinone

  • Aghapour, Ghasem;Mohamadian, Samaneh
    • Bulletin of the Korean Chemical Society
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    • 제33권4호
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    • pp.1209-1212
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    • 2012
  • In spite of many reports in the literature concerning with oxidation of benzylic alcohols to carbonyl compounds with 2,3-dichloro-5,6-dicyanobenzoquinone (DDQ) in stoichiometric amounts or even more, we surprisingly found that benzylic alcohols are directly oxidized to oximes using a catalytic amount of DDQ in the presence of hydroxylamine hydrochloride under solvent-free conditions. The present tandem catalytic method can be efficiently used for preparation of oximes in the presence of some other functional groups with excellent chemoselectivity.

초임계 건조에 의한 실리카 에어로겔의 저압 합성 (Low Pressure Synthesis of Silica Aerogels by Supercritical Drying)

  • 김동준;현상훈
    • 한국세라믹학회지
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    • 제33권5호
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    • pp.485-494
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    • 1996
  • Silica Aerogels with the density and porosity of 0.1g/cm3 and 96% were synthesized by two different supercri-tical drying processes (i.e additional solvent and intial pressure methods) Isoptopanol was chosen as sol-gel and supercritical drying solvents in order to synthesize aerogels at the lower temperature and pressure because the critical values of isopropanol are lower than those of methanol and ethanol commonly used. The P-V-T relationship of isopropanol was experimentally described for optimizing supercritical drying conditions such as the amount of extra solvent and supercritical drying temperature and pressure. In the addional solvent method monolithic and transparent aerogels were obtained by supercritical drying at 25$0^{\circ}C$ and 900 psing after 40% of the reactor volume was filled with isopropanol. Crack-free aerogels were synthesized at 25$0^{\circ}C$ and 1100~1200 psig by the initial pressure method with an intial nitrogen gas pressure of 400 psig and the isopropanol amount of 5% of the reactor volume.

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Styryl-6-Methoxy-2-Naphthyl Ketone 유도체의 합성 및 특성 분석 (Synthesis, Characterization and Correlation Analysis in Styryl 6-Methoxy-2-Naphthyl Ketones)

  • Thirunarayanan, G.
    • 대한화학회지
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    • 제51권2호
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    • pp.115-124
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    • 2007
  • α, β-불포화 케톤 유도체를 실리카-황산 촉매 하에서 비용매 교차 알돌 응축 반응법을 이용하여 합성하였다. 합성 수율은 90% 이상이었으며, 사용된 촉매는 회수 가능하였다. 합성돤 화합물들의 물리화학적인 특성은 IR, NMR, Mass 등의 분광학적 분석 방법을 이용하여 결정하였다. 케톤 생성물에 미치는 치환기 효과는 측정된 분광 데이터와 Hammet 치환기 상수간의 상관관계로 표현되는 다중 상관계수 방정식에 의하여 잘 설명될 수 있었다.

Preparation, Characterization and First Application of Alumina Supported Polyphosphoric Acid (PPA/Al2O3) as a Reusable Catalyst for the Synthesis of 14-Aryl-14H-dibenzo[a, j]xanthenes

  • Norouzi, Haniyeh;Davoodnia, Abolghasem;Bakavoli, Mehdi;Zeinali-Dastmalbaf, Mohsen;Tavakoli-Hoseini, Niloofar;Ebrahimi, Mahmoud
    • Bulletin of the Korean Chemical Society
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    • 제32권7호
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    • pp.2311-2315
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    • 2011
  • Alumina supported polyphosphoric acid (PPA/$Al_2O_3$) was successfully prepared by impregnation of alumina support by polyphosphoric acid and characterized using FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The catalytic behavior of this new solid acid supported heterogeneous catalyst was checked in the synthesis of 14-aryl-14H-dibenzo[a, j]xanthenes by cyclocondensation reaction of ${\beta}$-naphthol and aryl aldehydes under solvent-free conditions. The results showed that the novel catalyst has high activity and the desired products were obtained in very short reaction times with high yields. Moreover, the catalyst can be easily recovered by filtration and reused at least three times with only slight reduction in its catalytic activity.

Alumina Supported Ammonium Dihydrogenphosphate (NH4H2PO4/Al2O3): Preparation, Characterization and Its Application as Catalyst in the Synthesis of 1,2,4,5-Tetrasubstituted Imidazoles

  • Emrani, Anahita;Davoodnia, Abolghasem;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • 제32권7호
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    • pp.2385-2390
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    • 2011
  • Preparation of ammonium dihydrogenphosphate supported on alumina ($NH_4H_2PO_4/Al_2O_3$) and its primary application as a solid acid supported heterogeneous catalyst to the synthesis of 1,2,4,5-tetrasubstituted imidazoles by a one-pot, four-component condensation of benzil, aromatic aldehydes, primary amines, and ammonium acetate under thermal solvent-free conditions were described. The results showed that the novel catalyst has high activity and the desired products were obtained in high yields. Furthermore, the products could be separated simply from the catalyst, and the catalyst could be recycled and reused with only slight reduction in its catalytic activity. Characterization of the catalyst was performed by FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques.

PEG-Mediated Catalyst-Free Expeditious Synthesis of Functionalized Benzene/Biaryl and Fluoren-9-one Derivatives from Activated Acetylenes and 1,3-Diones

  • Piltan, Mohammad;Yavari, Issa;Moradi, Loghman;Zarei, Seyed Amir
    • 대한화학회지
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    • 제56권3호
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    • pp.316-321
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    • 2012
  • Poly(ethylene glycol) (PEG) has been used as a sustainable, non-volatile, and environmentally friendly reaction solvent for the synthesis of functionalized benzene/biaryl and fluoren-9-one derivatives from activated acetylenes and 1,3-diones at $100^{\circ}C$. No additional solvent and catalyst are required.