• Title/Summary/Keyword: Microwave assisted reaction

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Microwave-Assisted Cationic Ring-Opening Polymerization of Cyclic Imino Ethers

  • Hoogenboom Richard;Schubert Ulrich S.
    • Proceedings of the Polymer Society of Korea Conference
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    • 2006.10a
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    • pp.199-199
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    • 2006
  • Microwave-irradiation has become a common heat source in organic chemistry in the last decade. In recent years, polymer chemists also discovered the advances of microwave heating that include fast and efficient heating as well as the homogeneous heat profile and the easy access to pressurized reaction conditions. In this contribution, we report our investigations on the cationic ring-opening polymerization of 2-oxazolines that lead to a tremendous acceleration from several days to several minutes polymerization time. In addition, the optimized microwave-assisted polymerization procedure was applied for the preparation of libraries of diblock and triblock copolymers that were used for the determination of structure-property relationships in poly(2-oxazoline)s.

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Microwave-Assisted Solvent and Catalyst Free Synthesis of 2H-Pyrans

  • Edayadulla, Naushad;Lee, Yong Rok
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.2963-2967
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    • 2013
  • This paper describes a simple and efficient method involving domino Knovenegal/$6{\pi}$ electrocyclization for the preparation of a variety of 2H-pyrans using microwave irradiation under solvent- and catalyst-free conditions. This method offers the advantages of a green approach, high yields, and short reaction times. Sixteen compounds (9a-p) were obtained in good to excellent yields using the procedure.

Combustion Characteristics of Benzene over $LaMnO_3$ Perovskite-type Catalysts Prepared Using Microwave-assisted Process (마이크로파 공정으로 제조된 $LaMnO_3$ 페롭스카이트형 촉매에서 벤젠의 연소반응)

  • Jung, Won Young;Hong, Seong-Soo
    • Applied Chemistry for Engineering
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    • v.24 no.5
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    • pp.507-512
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    • 2013
  • Perovskite-type oxides were successfully prepared using microwave-assisted process, and by XRD, XPS, BET, and $H_2-TPR$. Their catalytic activities for the combustion of benzene were also examined. Most of catalysts studied showed the perovskite crystalline phase with the particle size of 21~35 nm. The $LaMnO_3$ catalyst showed the highest activity and the conversion reached almost 100% at $250^{\circ}C$. The catalysts prepared by microwave-assisted process showed higher activity compared to those prepared sol-gel method. In addition, the catalytic activity was increased with an increase of calcination temperature of $LaMnO_3$-type catalyst. The TPR results on the measurement of redox property showed a good correlation with the order of catalytic activity on the benzene combustion reaction.

Synthesis and characterization of AlN nanopowder by the microwave assisted carbothermal reduction and nitridation (CRN)

  • Chun, Seung-Yeop;Chun, Myoung-Pyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.5
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    • pp.223-228
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    • 2017
  • Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.

Microwave-assisted Synthesis of 2H-Benzo[b][1,4]oxazin-3(4H)-ones and 1H-Pyrido[2,3-b][1,4]oxazin-2(3H)-ones via Smiles Rearrangement

  • Hua, Zuo;Kam, Kyeong-Hee;Kwon, Hee-Jin;Meng, Lijuan;Ahn, Chul-Jin;Won, Tae-Jin;Kim, Tae-Hyun;Reddy, Ch. Raji;Chandrasekhar, S.;Shin, Dong-Soo
    • Bulletin of the Korean Chemical Society
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    • v.29 no.7
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    • pp.1379-1385
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    • 2008
  • Highly efficient synthesis of substituted benzo[1,4]oxazin-3-ones and pyrido[1,4]oxazin-2-ones under microwave irradiation via Smiles rearrangement is reported. Substituted benzo[1,4]oxazin-3-ones and pyrido[1,4]oxazin-2-ones were obtained by treatment of substituted 2-chlorophenols or 2-chloropyridols with N-substituted 2-chloroacetamide in the presence of potassium carbonate in MeCN and subsequent exposure to cesium carbonate in DMF. All the reactions which take 2-10 hours under conventional condition were completed successfully within a few minutes under microwave irradiation giving moderate to excellent yields.

Microwave Assisted Reaction of Condensed Thiophenes With Electron Poor Olefins

  • Al-zaydi, Khadijah M.;Elnagdi , Mohamed H.
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.591-596
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    • 2003
  • Aminothienopyridazines 1a, b and aminothienocoumarin 2 condensed with DMFDMA to yield amidines 3a, b and 4. These compounds reacted with N-phenylmaleimide to yield 9 and 10. On the other hand reacting 3a, b, 4, 18, 19 and 20 with maleic anhydride afforded only the formylated derivatives 5a, b, 6, 21, 22 and 23 respectively. The reaction of 3a, b with diethyl fumarate afforded 11, formed most likely via hydrolysis of the amidine 14 during working up the reaction mixture. Irradiation of N-phenylmaleimide in microwave oven afforded [2+2] and [2+2+2] cycloaddition product.

A Novel Route to New Bis(benzopyrano) Fused Dihydropyridines Using Dry Media

  • Kidwai, Mazaahir;Rastogi, Shweta;Mohan, Richa
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.119-121
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    • 2004
  • A new and efficient synthesis of the novel bioactive bis(benzopyrano) fused dihydropyridines is described. The conventionally developed route is a two step multicomponent condensation reaction. This is latter modified by a one pot microwave (MW) assisted reaction using inorganic solid support via the arylidene derivative intermediate. With this environmentally benign approach, the reaction time is brought down from hours to minutes along with a yield enhancement. Furthermore, the role of different solid supports is studied and it is concluded that the acidic alumina is the best solid support for the present investigation.

Microwave-Assisted and Conventional Synthesis of Benzothieno [3,2-e] [1,3,4] triazolo[4,3-c]pyrimidines: A Comparative Study

  • Gaonkar, Santhosh L.;Ahn, Chuljin;Princia, Princia;Shetty, Nitinkumar S.
    • Journal of the Korean Chemical Society
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    • v.58 no.4
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    • pp.388-392
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    • 2014
  • Benzothieno[2,3-d]pyrimidines (2,3,4) and benzothieno[3,2-e][1,3,4]triazolo[4,3-c] pyrimidines (5a-c) were synthesized from the precursor 2-amino-7-oxo-4,5,6,7-tetrahydro-1-benzothiophene-3-carbonitrile 1 by employing the conventional method as well as the microwave irradiation technique. The precursor 2-amino-3-cyanothiophene analogue 1 was synthesized by employing the well-known Gewald reaction. In the present work it has been found that the microwave supported syntheses are more efficient than the conventional classical heating methods. The structures of all the compounds were ascertained by spectral and analytical data.

Microwave-mediated Asymmetric Hydrogen Transfer by SBA-15-supported Ruthenium Catalyst (SBA-15 실리카에 고정화된 ruthenium 촉매를 사용한 Microwave하에서의 비대칭 수소 전달반응)

  • Jin, Myung-Jong;Jun, In-Chul
    • Korean Chemical Engineering Research
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    • v.46 no.4
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    • pp.752-755
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    • 2008
  • Mesoporous SBA-15 silica-supported TsCHDA and TsDPEN ligands have been prepared by reaction of SBA-15 silica with (1R,2R)-N-(trimethoxysilylpropyl-N-sulfonyl)-1,2-cyclohaxanediamine or (1R,2R)-N-(trimethoxysilylpropyl-N-sulfonyl)-1,2-diphenylethylenediamine-1,2-diphenylethylenediamine, respectively. The Ru complexes exhibited excellent catalytic activity and satisfactory enantioselectivity in the asymmetric hydrogen transfer of ketones under microwave conditions. The heterogeneous Ru catalyst was reusable as well as air-stable to allow easy use. Microwave-assisted efficient procedure has been developed for asymmetric hydrogen transfer.

Production of Chitosan from Crabshells using Microwave (마이크로파를 이용한 게껍질로부터 키틴/키토산 분리제조반응)

  • Choi, Guang Jin
    • Clean Technology
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    • v.7 no.4
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    • pp.281-290
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    • 2001
  • A microwave-assisted process to prepare chitosan from natural crabshells has been investigated. This study was primarily to examine the effectiveness of microwave as clean energy for chitosan preparation. Several human-edible organic acids were used as clean catalyst, possibly to improve the current HCl-based hydrolysis process of polymeric chitosan. The microwave was found to be effective substantially in reducing the reaction time. Nonetheless, no beneficial effect of microwave other than time, such as the chemical selectivity, was hardly observed. The organic acids were very effective in the hydrolysis reaction of polymeric chitosan. Their catalytic behavior was greatly improved especially when reactions were performed under pressure. In the case of autoclave reaction for 60 minutes at $120^{\circ}C$, viscous solution of polymeric chitosan (mol. wt. > 300,000) turned into thin solutions of water-like viscosity, which means chitosan molecules were decomposed to very small-sized oligomers.

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