• Title/Summary/Keyword: $C_2H_5OH$

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Nucleophilic Reaction of 2-Phenyl-4-quinolones with Methyl Iodide and Preparation of Its Derivatives (2-Phenyl-4-quinolones와 Methyl Iodide의 친핵반응에 의한 유도체의 합성)

  • Oh, Mi-Jung;Park, Myung-Sook
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.514-519
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    • 2008
  • We developed a convenient synthetic route to 3-alkylated 2-phenyl-4-quinolone derivatives (4a-h and 5a-c), which were expected to retain antitumor activity. A series of 2,3-dihydro-2-hydroxy-2-phenyl-4-quinolones (3a-h) was synthesized through dehydration, dealcoholation and hydration using acid-catalyzed one-pot reaction from anilines and ethyl benzoylacetates. 3-Methyl (or 3,3-dimethyl)-2-phenyl-4-quinolone derivatives 4 and 5 were synthesized from 3a-h through the methylation using methyl iodide. Formation of quinolone nucleus was undertaken with p-toluenesulfonic acid (p-TSA) at $90{\sim}110^{\circ}C$ in toluene for 3${\sim}$7.5 hr over the Dean-Stark apparatus. The key intermediates in these preparations are ${\beta}$-ketoesters 2a-h, which can be readily obtained from the corresponding anilines 1a-e by reaction with ethyl bezoylacetates.

Preparation of Spherical Gadolinium Compound Particles (구형 가돌리늄화합물 입자 제조)

  • 김응호;최청송;정경채;박진호;장인순
    • Journal of the Korean Ceramic Society
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    • v.30 no.7
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    • pp.563-570
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    • 1993
  • Spherical, monosized gadolinium compound was prepared by the reaction of Gd(NO3)3 solution with decomposition products of urea in the solution at evaluated temperature. Chemical composition and calcination characteristics of spherical gadolinium compound prepared were investigated by X-ray IR and TG-DTA. The approximate chemical composition of the spherical particle precipitated was Gd(OH)CO3.1.5H2O. Gd(OH)CO3.1.5H2O was calcined to monoclinic type Gd2O3 at 115$0^{\circ}C$ via cubic type Gd2O3 near $600^{\circ}C$. The effects of various parameters such as pH, temperature, concentration ratio of urea to gadolinium precusor, ageing time, and others material (CCl3COOH and HOCNH2) in stead of urea as precipitating agent on the properties of the resulting precipitates were studied systematically.

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Solvent Mediated Hydrogen-bonded Supramolecular Network of a Cu(II) Complex Involving N2O Donor Ligand and Terephthalate (N2O 주개 리간드와 테레프탈레이트를 포함하는 구리(II) 착물의 용매를 매개로 한 수소결합형 초분자 네트워크)

  • Chakraborty, Jishnunil
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.199-203
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    • 2011
  • The title one-dimensional hydrogen-bonded coordination compound $[Cu^{II}(C_{13}H_{17}N_3OBr)(C_8H_5O_4)]{\cdot}2H_2O.CH_3OH$ has been synthesized and characterized by single crystal X-ray diffraction study. The monomeric unit contains a square-planar $Cu^{II}$ centre. The four coordination sites are occupied by a tridentate anionic Schiff base ligand (4-bromo-2-[(2-piperazin-1-yl-ethylimino)-methyl]-phenol) which furnishes an $N_2O$-donor set, with the fourth position being occupied by the oxygen atom of an adjacent terephthalate unit. Two adjacent neutral molecules are linked through intermolecular N-H---O and O-H---N hydrogen bonds and generate a dimeric pair. Each dimeric pair is connected with each other via discrete water and methanol molecules by hydrogen bonding to form a one-dimensional supramolecular network.

Development of Biologically Active Compounds from Edible Plant Sources XXII. Isolation of Indoles from the Roots of Brassica campestris ssp rapa and their hACAT Inhibitory Activity (식용식물자원으로부터 활성물질의 탐색 XXII. 순무(Brassica campestris ssp rapa) 뿌리로부터 인돌 화합물의 분리 및 hACAT 저해 활성)

  • Bang, Myun-Ho;Lee, Dae-Young;Oh, Young-Jun;Han, Min-Woo;Yang, Hye-Joung;Chung, Hae-Gon;Jeong, Tae-Sook;Lee, Kyung-Tae;Choi, Myung-Sook;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.51 no.1
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    • pp.65-69
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    • 2008
  • The roots of Brassica campestris ssp rapa were extracted with 80% aqueous MeOH, and the concentrated extract was partitioned with EtOAc, n-BuOH and $H_2O$. From the EtOAc fraction, three compounds were isolated through the repeated silica gel and octadecyl silica gel (ODS) column chromatography. From the results of spectroscopic data including NMR and MS, the chemical structures of the compounds were determined as caulilexin C (1), indoleacetonitrile (2) and arvelexin (3). The arvelexin (3) has been isolated from this plant for the first time. Compounds 1, 2 and 3 showed inhibitory activity on human Acyl CoA: cholesterol. transferase 1 (hACAT1) by $54.6{\pm}6.0%$, $69.2{\pm}4.7%$ and $68.6{\pm}3.7%$, and on human Acyl CoA: cholesterol transferase 2(hACAT2) by $4.8{\pm}13.4%$, $45.6{\pm}4.8%$ and $39.5{\pm}4.3%$, respectively, at 100 ${\mu}g/ml$.

A Study of the Structure and Thermal Property of $Cu^{2+}\;and\;NH_{4}{^+}$ Ion-Exchanged Zeolite A

  • Park, Jong-Yul;Kang, Mi-Sook;Choi, Sang-Gu;Kim, Yang;Kim, Un-Sik
    • Bulletin of the Korean Chemical Society
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    • v.15 no.5
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    • pp.341-346
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    • 1994
  • The frameworks of $(Cu(NH_3)_3OH^+)_x(NH_4^+)_{12-x}-A{\cdot} zH_2O$ which were prepared by the ion-exchange of zeolite A with ammoniac cupric nitrate solution are more stable than those of $Cu_xNa_{12-2x} -A$ obtained by the ion exchange with aqueous cupric nitrate solution are more stable than those of $Cu_xNa_{12-2x} -A$ obtained by the ion exchange with aqueous cupric nitrate solution. An energetic calculation was made on the relatively stable $(CuOH^+)_2(NH_4^+)_{10}-A{\cdot} 2H_2O$ prepared by the partial evacuation of $(Cu(NH_3)_3OH^+)_2(NH_4^+)_{10}-A{\cdot} zH_2O$. The mean stabilization energies of water, OH-, and $NH_4^+$ ions are -30.23 kcal/mol, -60.24 kcal/mol, and -16.65 kcal/mol, respectively. The results of calculation were discussed in terms of framework stability. The $(Cu(NH_3)_3OH^+)_2(NH_4^+)_{10}-A{\cdot} zH_2O$ zeolite shows two step deammoniation reactions. The first deammoniation around 210 $^{\circ}$C (third DSC peak) was attributed to the decomposition of $[Cu(NH_3)_3OH^+]$ ion and the second one around 380 $^{\circ}$C (fourth DSC peak) was ascribed to the decomposition of $NH_4^+$ ion. The activation energies of the first and second deammoniation reactions were 99.75 kJ/mol and 176.57 kJ/mol, respectively.

Synthesis, Molecular and Microstructural Study of Poly-N-Vinylpyrrolidone Oximo-L-Valyl-Siliconate with IR, 1H-NMR and SEM

  • Singh, Man;Padmaja, G. Vani
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1869-1874
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    • 2010
  • By reducing PVP with $H_2NOH$.HCl and NaOH 2:2:1 mass ratios in aqueous ethanol, poly-N-vinyl pyrrolidone oxime [PVPO] was prepared with 92% yield. Applying the sol-gel concept, orthosilicic acid [OSA] was made by hydrolyzing TEOS with ethanol in 1:0.5 molar ratios using 1 N KOH aqueous solution as a catalyst. The OSA + PVPO + $_L$-Valine ($\alpha$-amino acid) were mixed with pure ethanolic medium in 1:2:2 mass ratios and refluxed at $78^{\circ}C$ and 6 pH for 6.5 h. A white residue of poly-N-vinyl pyrrolidone oximo-L-valyl-siliconate [POVS] appeared after 5 h. The heating of reaction mixture was stopped and the contents were brought to NTP. The residue formation of POVS was intensified with lowering a temperature and completely solidified within 5 h, was filtered using a vacuum pump with Whatmann filter paper no. 42. The residue of POVS was washed several times with 20% aqueous cold ethanolic solution and dried in vacuum chamber at $25^{\circ}C$ for 24 h. The MP was noted above $350^{\circ}C$. Structural and internal morphology were analyzed with IR and $^1H$-NMR, and SEM respectively. A drug loading and transporting ability of the POVS in water and at pH = 5 and 8 was determined chromatographically.

Flavonoids from Codonopsis lanceolata Leaves

  • Whang, Wan-Kyunn;Park, Kyun-Young;Chung, Sung-Hoon;Oh, In-Se;Kim, Il-Hyuk
    • Korean Journal of Pharmacognosy
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    • v.25 no.3
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    • pp.204-208
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    • 1994
  • For the investigation of resources in Codonopsis species, the studies were carried out to evaluate the pharmaco-constituents from the leaves of Codonopsis lanceolata (Campanulaceae) whose roots have been used to antitussive, expectorant, detoxicate, tonic, edible, etc. as a folk medicine in Korea. From the EtOAc and BuOH fractions of MeOH extract, three flavonoid compounds, $luteolin-7-O-{\beta}-_D-glucopyranoside$$(C_{21}H_{20}O_{1i},\;mp\;254{\sim}255^{\circ}$, compound 1), $luteolin-5-O-{\beta}-_D-glucopyranoside$$(C_{21}H_{20}O_{1i},\;mp\;279{\sim}281^{\circ}$, compound 2) and luteolin $(C_{15}H_{10}O_6,\;mp\;327{\sim}330^{\circ}$, compound 3) were isolated and identified on the basis of their physicochemical properties and spectroscopic evidences(UV, IR, $^1H-NMR$, $^{13}C-NMR$, MS etc.) in comparison with authentics respectively.

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Studies on Microbial Utilization of Agricultural Wastes (Part 4) Effect of Acid in Neutralization after Alkali Treatment of the Wastes on Cellulosic Single Cell Protein Production (농산폐자원의 미생물학적 이용에 관한 연구 (제사보) 기질처리시의 알칼이ㆍ산중화 조건에 대하여)

  • Lee, Gye-Jun;Ko, Young-Hee;Bae, Moo
    • Microbiology and Biotechnology Letters
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    • v.4 no.3
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    • pp.99-104
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    • 1976
  • Experiments were carried out to establish the effects of acids in neutralization after alkaline treatment of rice straw, with which cellulosic single cell protein can be produced by cellulose utilizing bacteria, Cellulomonas flavigena KIST 321, previously isolated by authors. Following results were obtained. 1. Rice straw as carbon source was pretreated with 10 volumes of 1 normality of NH$_4$OH or NaOH(NaOH/substrate:40%, and then washed with water or neutralized with H$_3$PO$_4$, H$_2$SO$_4$, HCl and CH$_3$COOH. Among the above mentioned methods, neutralization with H$_3$PO$_4$after alkaline treatment was proved to be the most effective on its digestibility and SCP production. Dry cell 12.28g/$\ell$ and 78% digestibility were obtained. 2. When rice straw was treated with NaOH solution, the result suggested that the productibity of cell-mass was attained on treatment of rice straw with 6% of NaOH (NaOH/substrate ratio) for 15~24hrs at room temperature. 3. When rice straw was treated with NaOH, a volume of water to substrate is adequate by two or three fold and the amount of NaOH can be economized up to 5% for the weight of rice straw. 4. The steaming of rice straw at 121$^{\circ}C$ for 30min. in alkaline treatment of rice straw gave the similiar effectiveness to that at room temperature for 15~24hrs. and accelerated the sterilization of the substrate. 5. Finally, the level of inorganic phosphate in a medium was investigated. 11.2g of dry cell was produced at the concentration of 0.2%, phosphate (phosphorous level 0.04%) in medium even though treated rice straw was neutralized with HCI instead of H$_3$PO$_4$, and 12.2g/$\ell$ at the concentration of 0.3% phosphate (phosphorous 0.04%) on neutralization with H$_2$SO$_4$.

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Kinetic Studies on the Oxidation of Oxalate Complex of Oxomolybdenum (V) of Hydrogen Chromate Ion (수소크롬산 (VI) 이온에 의한 몰리브덴 (V) 의 옥살산착물의 산화반응)

  • Chang-Yong Kwon;Chang-Su Kim
    • Journal of the Korean Chemical Society
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    • v.30 no.2
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    • pp.231-236
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    • 1986
  • Oxidation of $[Mo_2O_4(C_2O_4)_2(OH_2)_2]^{2-}$ with hydrogen chromate yields the molybdenum (VI) complex, $[Mo_2O_4(C_2O_4)_2(OH_2)_2]^{2-}$. Stoichiometry for the reaction of $[Mo_2O_4(C_2O_4)_2(OH_2)_2]^{2-}$ with hydrogen chromate are expressed as ${3Mo_2}^V+2Cr^{VI}\;{\rightleftharpoons}\;{3Mo_2}_{VI}+2Cr^{III}$. Observed rate constants are dependent on $[H+]^2$. The kinetic data are consistent with a mechanism in which three successive single-electron steps convert $Cr^{VI}$to $Cr^{III}$ by way of intermediate Cr^V$ and $Cr^{IV}$. Mechanism of the reaction are presented and discussed.

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Hydrated Form of 4-N,N-Dimethylamino-4'-N'-Methyl-Stilbazolium Tosylate, $C_{16}H_{19}N_2(C_7H_7SO_3{\cdot}H_2O)$ (4-N,N-Dimethylamino-4'-N'- Mothy1-stilbazolium tosylate의 수화물)

  • Hong Hyung-Ki;Yoon Choon Sup;Suh Il-Hwan;Lee Jin-Ho;Choi Sung-San;Oh Mi-Ran;Marder Seth R.
    • Korean Journal of Crystallography
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    • v.8 no.1
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    • pp.1-5
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    • 1997
  • The crystal structure of the title compound consists of discrete 4-N,N-dimethylamino-4'-N'-methyl-stilbazolium, $C_{16}H_{19}N_2$, and tosylate, $C_7H_7SO_3$, dimer. The 4-N,N-dimethylamino-4'-N'-methyl-stilbazolium molecule has a trans conformation at the central C=C double bond: the dihedral angle between the phenyl and the pyridyl rings is $5.7(2)^{\circ}$ and the whole molecule is planar within $0.138(8){\AA}$. Tosylate molecules display hydrogen-bonded dimers with the O-H...O distances of 2.855(9) and $2.899(8){\AA}$, respectively. The shortest intermolecular contact is the distance $3.10(1){\AA}$ between O(3) and C(16).

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