• 제목/요약/키워드: refluxing

검색결과 87건 처리시간 0.021초

Optimization of the Reaction Conditions for Synthesis of 3-(Aryloxy)quinoline Derivatives via Friedländer's Cyclization Reaction

  • Khan, Mohammad Ashrafuddin;El-Gamal, Mohammed I.;Oh, Chang-Hyun
    • Bulletin of the Korean Chemical Society
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    • 제34권6호
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    • pp.1848-1852
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    • 2013
  • 6,7-Dimethoxy-2-methyl-3-(4-nitrophenoxy)quinoline was synthesized by Friedl$\ddot{a}$nder's cyclization reaction. Different bases and solvents were tested in order to optimize the reaction conditions. The highest yields were obtained using piperidine in refluxing ethanol. Further reactions were carried out in order to prepare different diarylamide and diarylurea derivatives in moderate to high yields in order to examine their anticancer activities.

3-멀?토-4H-피롤로피리딘의 합성 (Synthesis of 3-mercapto-4H-pyrrolopyridine)

  • 마은숙
    • 약학회지
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    • 제46권6호
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    • pp.369-374
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    • 2002
  • Dilithiation of 4-(pivaloylamino)pyridine (5) followed by reaction with tetraisopropylthiuram disulfide(TITD) gave rise to 3-(diisopropyldithiocarbamato)-4-(pivaloylamino)pyridine (6). 3-Mercapto-4H-pyrrolopyridine(2) was synthesized from compound 6 by two methods. The first method was that compound 6 was treated with 5M-HCl to form 2-t-butylthiazolo[5,4-c]pyridine (7) and hydrolysed in refluxing 10% NaOH and solid NaOH to prepare bis(4-amino-3-pyridyl)disulfide (8). And compound 8 was reacted with 2,5-dimethoxytetrahydrofuran and NaBH$_4$ to afford compound 2. The second method was that compound 6 was hydrolysed with 10% NaOH and followed to react with 2,5-dimethoxytetrahydrofuran to form compound 11. And then compound 11 was treated with 20% ethanolic KOH solution to synthesize compound 2.

수지 코팅에 의한 리튬이온전지용 탄소 부극재료의 전지 성능 개선 (Enhancement of the Cell Performance for an Carbon Anode in Li-ion Battery)

  • 김정식;윤휘영;유광수
    • 한국세라믹학회지
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    • 제38권8호
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    • pp.755-760
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    • 2001
  • 본 연구에서는 카본전극의 표면개질에 따른 리튬이온 전지의 전지특성 변화에 대해서 연구하였다. 즉, mesocarbon microbeads(MCMB) 카본에 에폭시 수지(resin)를 코팅시킴으로서 카본전극 표면에 개질시켰으며, 이에 따른 전극의 전기화학적 특성을 고찰하였다. 에폭시 수지에 의한 카본의 표면코팅은 30%의 H$_2$SO$_4$용액에서 2시간 동안 refluxing한 MCMB를 에폭시 수지를 용해시킨 THF(tetrahydrofuran) 용액에 넣어 혼합함으로써 MCMB 표면에 에폭시 수지가 코팅되도록 하였다. 이렇게 에폭시 수지가 코팅된 MCMB를 약 1000-130$0^{\circ}C$로 열처리하여 고분해능 투과전자현미경으로 관찰한 결과, 코팅층은 비정질 카본 구조를 갖게됨을 알 수 있었다. 또한, 에폭시 수지에 의하여 코팅된 MCMB는 코팅되지 않은 MCMB보다 더 높은 BET 비표면적을 나타내었다. Li/MCMB 전지 cell을 만들어 충방전시험을 수행한 결과, 에폭시 수지에 의하여 코팅된 MCMB로 만든 전극이 더 우수한 충방전 용량과 싸이클 특성을 나타내었다. 에폭시 수지 코팅으로 전극 표면을 개질시킴으로서 전지특성이 개선된 원인에 관하여 에폭시 코팅의 결정구조와 전극계면에서의 부동태 피막(passivation film) 형성과 연계하여 논의하였다.

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인삼제품의 Saponin 추출방법에 관한 연구 (Study on of Extraction Methods of Saponin in Ginseng Products)

  • 손현주;장진규
    • Journal of Ginseng Research
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    • 제8권1호
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    • pp.32-37
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    • 1984
  • In order to shorten the extraction time of saponin in ginseng products, election with Extrelut column and phase-separation methods were compared. The results obtained are as follows. 1. Saponin of ginseng products was extracted completely within 3 hours by election method with Extrelut column, and the rate of removing glucose by the column was increased with increasing glucose content in ginseng products. 2. Stirring method was superior to refluxing method for removing sugars from ginseng products, and removing rate was deceased in the order of lactose, sucrose and glucose. 3. Extraction rate of ginsenoside from ginseng extracts by the elution method was nearly same as that of phase-separation method; however, the former was much higher than the latter in the case of ginseng teas. Therefore, the elution by Extrelut column is to be improper for extraction of saponin in ginseng tea which contains much sugar. It was necessary to remove lipophilic compounds for extraction of saponin from ginseng extracts by elution with Extrelut column.

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Nickel-Catalyzed Coupling of Arenesulfonates with Primary Alkylmagnesium Halides

  • Cho, Chul-Hee;Sun, Myung-Chul;Park, Kwang-Yong
    • Bulletin of the Korean Chemical Society
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    • 제26권9호
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    • pp.1410-1414
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    • 2005
  • Neopentyl arenesulfonates reacted with primary alkylmagnesium halides in the presence of $(PPh_3)_2NiCl_2$ to produce the corresponding alkylarenes. The efficiency of this coupling reaction considerably depends on the nature of catalyst and solvent. Highest yield was obtained by using three equivalents of Grignard reagent to a mixture of $(PPh_3)_2NiCl_2$ and arenesulfonate in refluxing $Et_2O$. This reaction represents a novel method allowing the efficient and creative substitution of sulfur-containing groups in aromatic compounds. It also shows that the alkyloxysulfonyl group might be a suitable alternative to halides and triflate in some circumstances.

A New and Convenient Method for Reduction of Oximes to Amines with NaBH3CN In the Presence of MoCl5/NaHSO4·H2O System

  • Kouhkan, Mehri;Zeynizadeh, Behzad
    • Bulletin of the Korean Chemical Society
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    • 제32권9호
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    • pp.3323-3326
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    • 2011
  • Various aldoximes and ketoximes were efficiently reduced to their corresponding amines with $NaBH_3CN$ in the presence of $MoCl_5/NaHSO_4{\cdot}H_2O$ system. Reduction reactions were carried out in refluxing EtOH or DMF within 0.3-3.8 h to afford the amines in high to excellent yields.

야생 비늘 버섯의 항암 성분에 관한 연구 (Studies on Antitumor Components of Wild Pholiota squarrosa (Fr.) Quel.)

  • 박완희
    • 약학회지
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    • 제26권3호
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    • pp.185-188
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    • 1982
  • In order to investigate the antitumor components of Korean wild higher fungi, the carpo-phores of Pholiota squarrosa collected in Kaung Nung area were extracted with water by refluxing for eight hours at 80-90.deg. C. The extracts were dialized for six days against distilled water and lyophilized to produce crude polysaccharide powders. They were found to have the antitumor activity against sarcoma 180 implanted in mice. Especially, the inhibition ratio of the extract of Pholiota squarrosa was 78.7% in the dose of 20mg/kg/day for the period of ten days. The tumor in two of the ten mice was completely regressed. The components of these aqueous extracts were found to be polysaccharide and protein. The total polysaccharide was 42% by Anthrone method and the protein was 55% by Lowry-Folin method in the antitumor component of Pholiota squarrosa.

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One-Pot Synthesis of CdSe Quantum Dots Using Selenium Dioxide as a Selenium Source in Aqueous Solution

  • Wang, Yilin;Yang, Hong;Xia, Zhenyi;Tong, Zhangfa;Zhou, Liya
    • Bulletin of the Korean Chemical Society
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    • 제32권7호
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    • pp.2316-2318
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    • 2011
  • A novel technology has been developed for the synthesis of thioglycolic acid (TGA)-capped CdSe quantum dots (QDs) in aqueous medium. The reaction was carried out in air atmosphere with one-pot by using $SeO_2$ to replace Se or $Na_2Se$. The technological parameters including refluxing time, pH values and molar ratios of selenium to cadmium had significant influence on the luminescence properties of CdSe QDs. Furthermore, the obtained QDs were characterized by fluorescent spectroscopy, X-ray powder diffraction (XRD) and transmission electron microscopy (TEM), respectively. The results demonstrated that the CdSe QDs were of zinc-blended crystal structure in a sphere-like shape.

잠재적 COX-2 억제작용이 있는 1,5-Diarylhydantoin유도체의 합성 (Synthesis of Potential COX-2 Inhibitory 1,5-Diarylhydantoin Derivatives)

  • 권순경;박해선
    • 약학회지
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    • 제48권2호
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    • pp.135-140
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    • 2004
  • For the development of new COX-2 inhibitors, 1,5-diarylhydantoins 5a∼5c and 1,5-diaryl-2-thiohydantoin 6a∼6c were synthesized from commercially available phenylacetic acids through esterification, bromination, C-N bond formation and cyclization. Esters 2a∼c were efficiently synthesized from the starting materials 1a∼c by refluxing in absolute methanol for 3 hours with catalytic concentrated sulfuric acid. Bromination of 2a∼c was carried out with use of N-bomosuccinimide at rt in dichloromethane. The bromine of 3a∼c was substituted with aniline in ethanol or N,N-dimethylformamide to provide 4a∼c. Hydantoins and 2-thiohydantoins were synthesized from 4a∼c by treatment of potassium isocyanate or potassium thiocyanate in dil-ethanol with triethylamine.

Properties of Co-Ferrite Nanoparticles Synthesized by Thermal Decomposition Method

  • Oh, Young-Woo;Liu, J.P.
    • Journal of Magnetics
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    • 제11권3호
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    • pp.123-125
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    • 2006
  • Co-ferrite nanoparticles have been synthesized by the decomposition of iron(III) acetylacetonate, $Fe(acac)_3$ and Co acetylacetonate, $Co(acac)_2$ in benzyl/phenyl ether in the presence of oleic acid and oleyl amine at the refluxing temperature of $295^{\circ}C$/$265^{\circ}C$ for 30 min. before cooling to room temperature. Particle diameter detected by PSA can be turned from 4 nm to 20 nm by seed-mediated growth and reaction conditions. Structural and magnetic characterization of Co-ferrite were measured by use of HRTEM, SAED (selected area electron diffraction), XRD and SQUID. The as-synthesized Co-ferrite nanoparticles have a cubic spinel structure and coercivity of 20 nm $CoFe_{2}O_{4} nanoparticles reached 1 kOe at room temperature and 18 kOe at 10 K.