• 제목/요약/키워드: Microwave-assisted synthesis

검색결과 59건 처리시간 0.028초

MeO-PEG-OMe를 사용한 benzo-[1,4]-oxazinone 화합물의 마이크로웨이브 합성 (Microwave-assisted Synthesis of Benzo-[1,4]-oxazinones Using MeO-PEG-OMe as Solvent)

  • 임재민;감경희;김신형;장기완;신동수
    • 대한화학회지
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    • 제56권4호
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    • pp.468-472
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    • 2012
  • 마이크로웨이브를 이용한 가열 방법과 MeO-PEG-OMe를 용매로 사용하여, benzo-[1,4]-oxazinone의 효율적인 one-pot 합성방법을 개발하였으며, 개발한 합성방법을 이용하여, 8 가지의 benzo-[1,4]-oxazinone 화합물과 1H-pyrido[2,3-b][1,4]-oxazin-2-(3H)-one을 좋은 수율로 합성하였다.

Clean and Efficient Synthesis of Furfural From Xylose by Microwave-Assisted Biphasic System using Bio-Based Heterogeneous Acid Catalysts

  • Vo, Anh Thi Hoang;Lee, Hong-shik;Kim, Sangyong;Cho, Jin Ku
    • 청정기술
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    • 제22권4호
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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.

One Pot Synthesis of Novel Cyanopyridones as an Intermediate of Bioactive Pyrido[2,3-d]Pyrimidines

  • Khatri, Taslimahemad T.;Shah, Viresh H.
    • 대한화학회지
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    • 제58권4호
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    • pp.366-376
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    • 2014
  • Synthesis, structural characterization, and biological activity studies of novel pyrido[2,3-d]pyrimidines (10a-h, 11a-h) are described. Cyclization of cynoacetamides (4, 5) with malonitrile (7) and aldehyde (6a-h) via Hantzsch pyridine synthesis afforded cyanopyridones (8a-h, 9a-h), which on cyclization with formic acid under microwave conditions led to the final product. All the reactions are significantly faster and the isolated yields are remarkably higher in microwave conditions compared to the conventionally heated reactions. The compounds were tested in vitro for their antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Bacillus subtillus, Staphylococcus aureus, and Micrococcus luteus and antifungal activity against Trichphyton longifusus, Candida albicans, Microsporum canis, Fusarium solani. Compounds 10b, 10e, 11b and 11e exhibited good antibacterial and antifungal activities compared with standards.

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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    • 제29권7호
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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.

Effect of microwave irradiation on lipase-catalyzed reactions in ionic liquids

  • An, Gwangmin;Kim, Young Min;Koo, Yoon-Mo;Ha, Sung Ho
    • 분석과학
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    • 제30권3호
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    • pp.138-145
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    • 2017
  • Microwave-assisted organic synthesis has gained a remarkable interest over the past years because of its advantages - (i) rapid energy transfer and superheating, (ii) higher yield and rapid reaction, (iii) cleaner reactions. Ionic liquids are well known for their unique properties such as negligible vapor pressure and high thermal stability. With these properties, ionic liquids have gained increasing attention as green, multi-use reaction media. Recently, ionic liquids have been applied as reaction media for biocatalysis. Lipase-catalyzed reactions in ionic liquids provide high activity and yield compared to conventional organic solvents or solvent free system. Since polar molecules are generally good absorbent to microwave radiation, ionic liquids were investigated as reaction media to improve activity and productivity. In this study, therefore, the effect of microwave irradiation in ionic liquids was investigated on lipase catalyzed reactions such as benzyl acetate synthesis and caffeic acid phenethyl ester synthesis. Comparing to conventional heating, microwave heating showed almost the same final conversion but increased initial reaction rate (3.03 mM/min) compared to 2.11 mM/min in conventional heating at $50^{\circ}C$.

Solid-state metathetic synthesis of MWO4 (M=Zn, Co) particles assisted by microwave irradiation

  • Lim, Chang-Sung
    • 한국결정성장학회지
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    • 제20권6호
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    • pp.295-300
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    • 2010
  • Metathetic route for the $MWO_4$ (M=Zn, Co) particles is a simple method of synthesis and a viable alternative method in a short time. $MWO_4$ (M=Zn, Co) particles were synthesized using solid-state metathetic (SSM) method with microwave irradiation. The $MWO_4$ (M=Zn, Co) particles were formed completely at $600^{\circ}C$ for 3 h. The crystallization process, thermal decomposition and morphology of the $MWO_4$(M= Zn, Co) particles were evaluated. The characteristics of the SSM reaction and the formation of a high lattice energy by-product NaCl were discussed.

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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    • 제34권10호
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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.