• 제목/요약/키워드: Active methylene group

검색결과 15건 처리시간 0.027초

Silica Supported Ammonium Acetate: An Efficient and Recyclable Heterogeneous Catalyst for Knoevenagel Condensation between Adehydes or Ketones and Active Methylene Group in Liquid Phase

  • Gupta, Raman;Gupta, Monika;Paul, Satya;Gupta, Rajive
    • Bulletin of the Korean Chemical Society
    • /
    • 제30권10호
    • /
    • pp.2419-2421
    • /
    • 2009
  • A simple and efficient method has been developed for Knoevenagel condensation between aldehydes or ketones and active methylene group by stirring in methylene chloride at 60 ${^{\circ}C}$ under heterogeneous conditions using silica supported ammonium acetate. The products are obtained in excellent yields and are in a state of high purity. The structures of the products were confirmed by IR, $^1H$ NMR and mass spectral data and comparison with authentic samples available commercially.

Methylene Blue-stained Interstitial Cells are Electrically Active in the Myenteric Board Freshly Prepared from the Murine Small Intestine

  • Lee, Kyu-Pil;Jeon, Ju-Hong;So, In-Suk;Kim, Ki-Whan
    • The Korean Journal of Physiology and Pharmacology
    • /
    • 제10권4호
    • /
    • pp.193-198
    • /
    • 2006
  • Many gastrointestinal muscles show electrical oscillation, so-called 'slow wave', originated from interstitial cells of Cajal (ICCs). Thus, a technique to freshly isolate the cells is indispensable to explore the electrophysiological properties of the ICCs. To apply an enzyme solution on the serosal surface for cell isolation, the intestine was inverted and 0.02% trypsin solution and 0.04% collagenase solution were applied to serosal cavity. After the enzyme treatment, mucosal layer was removed and longitudinal muscle layer was gently separated from the rest of tissue. The thin layer was stretched in the recording chamber and mounted on an inverted microscope. Using ${\beta}-escine$, perforated whole cell patch clamp technique was used. Under a microscope, the tissue showed smooth muscle cells and interstitial cells around the myenteric plexus. Under voltage clamp condition, three types of membrane potential were recorded. One group of interstitial cells, which were positive to methylene blue and CD34, showed spontaneous outward current. These cells had bipolar shape and were considered as fibroblast-like cells because of their peculiar shape and arrangement. Another group, positive to c-kit and methylene blue, showed spontaneous inward current. These cells had more rounded shape and processes and were considered as ICCs. The third, positive to c-kit and had granules containing methylene blue, showed quiet membrane potentials under the voltage-clamp mode. These cells appeared to be resident macrophages. Therefore, in the freshly isolated thin tissue preparation, methylene blue could easily identify three types of cells rather than morphological properties. Using this method, we were able to study electrical properties of fibroblast and residential macrophage as well as myenteric ICCs.

Synthesis and Absorption Spectral Properties of Bis-methine Dyes Exemplified by 2,5-Bis-arylidene-1-dicyanomethylene-cyclopentanes

  • Asiri, Abdullah Mohamed
    • Bulletin of the Korean Chemical Society
    • /
    • 제24권4호
    • /
    • pp.426-430
    • /
    • 2003
  • A range of methine dyes has been synthesized by condensation of highly electronegative active methylene compound dicyanomethylenecyclopentane derived from cyclopentanone with the formyl group of substituted benzaldehydes. The electronic absorption spectroscopic properties of the dyes were investigated. In general, substituents on the aromatic aldehyde moiety have a significant effect on the visible absorption maxima of the dyes; increasing the solvent polarity also showed a pronounced effect on the absorption maxima.

Straightforward synthesis of 4'${\alpha}$-C-hydroxymethyl branched novel carbocyclic nucleosides

  • Oh, Jung-Hyo;Kim, Kwan-Woo;Hong, Joon-Hee
    • 대한약학회:학술대회논문집
    • /
    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
    • /
    • pp.354.1-354.1
    • /
    • 2002
  • Carbocyclic nucleosides are unique class in which a methylene group replaces the oxygen in the furan, which result in metabolic stability to endogenous phosphorylase. The biologically active natural carbocyclic nucleosides such as aristeromycin and neplanocin were found to possess interesting biological properties including antiviral and antitumor activity. (omitted)

  • PDF

시판 기능성식품으로부터의 실데나필 유도체 부정첨가물질의 분리 및 구조규명 (Isolation and Identification of an Unauthorized Sildenafil Analogue in a Commercial Functional Food)

  • 백두종
    • 대한화학회지
    • /
    • 제54권4호
    • /
    • pp.443-446
    • /
    • 2010
  • 기능성식품으로 시판되는 건강음료를 HPLC 분석한 결과 발기부전치료제로 허가받은 비아그라$^{(R)}$의 활성주성분인 실데나필과 구조적으로 유사한 부정첨가물질이 발견되었다. 이 부정첨가물질의 구조를 규명하기 위해 건강음료를 methylene chloride로 추출한 다음 그 추출물을 semipreparative HPLC로 정제하였다. 분리된 물질의 화학구조는 IR, LC/MS-ESI, NMR 분광학으로 규명하였는데 실데나필과 유사한 특징을 보였고 구조상의 유일한 차이는 실데나필의 methylpiperazine 부분구조를 부정첨가물질에서 hydroxyethylpiperazine으로 치환한 것이었다.

시판 기능성식품으로부터의 타다라필 유도체 부정첨가물질의 분리 및 구조규명 (Isolation and Identification of an Unauthorized Tadalafil Analogue in a Commercial Functional Food)

  • 백두종
    • 약학회지
    • /
    • 제54권4호
    • /
    • pp.240-243
    • /
    • 2010
  • High-performance liquid chromatography (HPLC) screening method revealed that a propolis product marketed as a functional food contained an undeclared substance similar to tadalafil, the active ingredient of the prescription drug Cialis$^{(R)}$ approved for the treatment of male erectile dysfunction. In order to identify the illegal additive, the propolis product was extracted with methylene chloride, and the extract was purified further using semipreparative HPLC. The chemical structure of the isolated substance was elucidated based on IR, LC/MS-ESI, and $^1H$- and $^{13}C$-NMR spectroscopy, which showed the characteristics similar to tadalafil. The only difference was the substitution of the methyl group at the piperazinedione ring of tadalafil to the amino group of the identified illegal additive.

Preparation of Dinuclear, Constrained Geometry Zirconium Complexes with Polymethylene Bridges and an Investigation of Their Polymerization Behavior

  • Noh, Seok-Kyun;Jiang, Wen-Long
    • Macromolecular Research
    • /
    • 제12권1호
    • /
    • pp.100-106
    • /
    • 2004
  • We have prepared the polymethylene-bridged, dinuciear, half-sandwich constrained geometry catalysts (CGC)[Zr(η$\^$5/:η$^1$-C$\_$9/H$\_$5/SiMe$_2$NCMe$_3$)]$_2$[(CH$_2$)$\_$n/][n=6(9), n=12(10)]by treating 2 equivalents of ZrCl$_4$with the corresponding tetralithium salts of the ligands in toluene. $^1$H and $\^$13/C NMR spectra of the synthesized complexes provide firm evidence for the anticipated dinuciear structure. In $^1$H NMR spectra, two singlets representing the methyl group protons bonded at the Si atom of the CGC are present at 0.88 and 0.64 ppm, which are considerably downfield positions relative to the shifts of 0.02 and 0.05 ppm of the corresponding ligands. To investigate the catalytic behavior of the prepared dinuciear catalysts, we conducted copolymerizations of ethylene and styrene in the presence of MMAO. The prime observation is that the two dinuclear CGCs 9 and 10 are not efficient for copo-lymerization, which definitely distinguishes them from the corresponding titanium-based dinuclear CGC. These species are active catalysts, however, for ethylene homopolymerization; the activity of catalyst 10, which contains a 12-methylene bridge, is larger than that of 9 (6-methylene bridge), which indicates that the presence of the longer bridge between the two active sites contributes more effectively to facilitate the polymerization activity of the dinuciear CGC. The activities increase as the polymerization temperature increases from 40 to 70$^{\circ}C$. On the other hand, the molecular weights of the polyethylenes are reduced when the polymerization temperature is increased. We observe that dinuciear metallocenes having different-length bridges give different polymerization results, which reconfirms the significant role that the nature of the bridging ligand has in controlling the polymerization properties of dinuclear catalysts.

Cyclohexane Oxidations by an Iron-Palladium Bicatalytic System; Soluble Catalysts and Polymer Supported Catalysts

  • 준기원;심은경;박상언;이규완
    • Bulletin of the Korean Chemical Society
    • /
    • 제16권5호
    • /
    • pp.398-400
    • /
    • 1995
  • Selective oxidation of cyclohexane in acetone solution has been studied using iron catalysts with hydrogen peroxide in-situ produced by palladium catalyst. Iron tetraphenylporphyrin chloride shows the highest activity among the tested chlorides and porphyrin complexes of some metals of the first transiton series. Iron chloride and iron tetraphenylporphyrin chloride were supported on four kinds of 4-vinylpyridine copolymer with styrene or divinyl-benzene. Nitrogen 1s photoelectron spectra give the evidence that pyridyl nitrogens of the 4-vinyl pyridine copolymer act as ligands to bind iron species. The copolymer with styrene is the most efficient support for the binding because its solubility in catalyst preparation solvent (methylene chloride) gives the pyridyl group advantage to contact with the iron catalysts. However, better catalytic activity per iron atom could be obtained with a rigid crosslinked polymer due to active site isolation.

Achromobacter Protease I (API)의 기질특이성 결정기의 동정과 변이체[D225E]의 Ornithine 기질에 대한 촉매활성 (Identification of Substrate Specificity Determinant of Achromobacter Protease I (API) and Catalytic Activity of Mutant D225E for Ornithine Substrate)

  • 임성일;권오진;최청
    • Applied Biological Chemistry
    • /
    • 제40권3호
    • /
    • pp.189-195
    • /
    • 1997
  • 부위특이적 변이제작을 통하여 Achromobacter protease I (API)의 lysin에 대한특이성의 구조적 근거를 조사하였다. Lysine 특이성을 결정하는 결정기로서 예상되는 잔기중의 하나인 Glu190을 glutamine, aspartic acid, leucine으로 치환하였을 경우, 전구체단백질은 Iysine 특이성을 가진 완전한 활성효소로서 발현되어 자기촉매적으로 processing되었다. 다른 하나의 잔기인 Asp225을 asparagine, leucine으로 치환한 변이체에서는 불활성 전구체인 pro-API으로서 발현되었으나, 변이체 (D225E)의 경우는 서서히 자기촉매적으로 maturation 되었다. 성숙체인 변이체 (D225E)의 Iysylendopeptidase 활성은 wild-type APl의 0.25%이였으며, 이 활성의 감소는 기질 Iysine과 효소와의 친화력 감소가 주 원인이었다. 이러한 결과로부터 Asp225가 Iysylendopeptidase의 엄격한 기질특이성에 결정적인 역할을 담당한다는 것이 시사되었다. 한편, 변이체 (D225E)는 ornithine 기질에 대해서 효소활성 이 검출되지 않았다. 이 변이체의 촉매잔기인 Ser194가 native API과 마찬가지로 DFP, PMSF와 근본적으로 동일한 반응성이 있는 것으로 나타나 225번 위치의 methylene 1 unit 더 긴 측사는 subsite P1의 methylene 1 unit 짧은 측사에 의해 보상되지 않는다는 것을 알 수 있었다.

  • PDF