• Title/Summary/Keyword: Direct Synthesis

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(-)-β-Narcotine: A Facile Synthesis and the Degradation with Ethyl Choroformate

  • Lee, Dong-Ung
    • Bulletin of the Korean Chemical Society
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    • v.23 no.11
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    • pp.1548-1552
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    • 2002
  • $(-)-\beta-Narcotine$ (6), a phthalideisoquinoline alkaloid, was synthesized conveniently by the direct condensation of cotarnine (1) and iodomeconine (2) prepared by aromatic iodination using thallium trifluoroacetate/KI and by the successive reduction of resulting $iodo-{\beta}-narcotine$ (5) with aluminum amalgam. Its structure including a stereochemistry was confirmed by instrumental analyses. This synthetic alkaloid was degraded with ethyl chloroformate at room temperature to afford the chloro-carbamate 6b as a crystalline intermediate, which was unexpectedly converted into the carbinol 8 by exchange of Cl with OH of water contained in the solvents and the ethoxy-carbamate 9, probably because of ethanol added to chloroform as a solvent stabilizer during the purification by column chromatography.

Synthesis of Aniline and Isoquinoline derivatives using Deamination and Nitration (Deamination과 Nitration반응을 이용한 아닐린과 Isoquinoline 유도체의 합성)

  • Yoon, Cheol-Hun;Lee, Ki-Chang
    • Journal of the Korean Applied Science and Technology
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    • v.15 no.2
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    • pp.49-57
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    • 1998
  • This study is to develop a new synthetic method for the nitroarenes via non-electrophilic substitution. Direct nitration at the C-1 position of isoquinoline has never been reported and substitution in isoquinoline under the normal nitration condition occurs at C-5 and C-8. We have demonstrated a facile one-step sythetic method for the nitration of isoquinolines at the C-1 position, which involves the electrophilic attack of a $DMSO-Ac_2O$ complex, followed by nucleophilic addition of nitrate ion to this intermediate. Since the reaction is simple and mild, this method has preparative merit since 1-nitroisoquinolines are not readily accessible by other methods. Application to the synthesis of poly nitroarenes from the corresponding anilines was also described.

Synthesis and Antiviral Activity Evaluation of 5',5'-Difluoro-2'-methylapiosyl Nucleoside Phosphonic Acid Analogs

  • Hong, Joon Hee
    • Journal of Integrative Natural Science
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    • v.8 no.3
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    • pp.153-163
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    • 2015
  • Racemic synthesis of novel 5',5'-difluoro-2'-methyl-apiose nucleoside phosphonic acid analogs was achieved as potent antiviral agents. Phosphonation was performed by direct displacement of triflate intermediate with diethyl (lithiodifluoromethyl) phosphonate to give the corresponding (${\alpha},{\alpha}$-difluoroalkyl) phosphonate. Condensation successfully proceeded from a glycosyl donor with persilylated bases to yield the nucleoside phosphonate analogs. Deprotection of diethyl phosphonates provided the target nucleoside analogs. An antiviral evaluation of the synthesized compounds against various viruses such as HIV, HSV-1, HSV-2 and HCMV revealed that the pyrimidine analogs (cytosine, uracil, and thymine) have weak anti-HIV or HCMV activity.

Transient Response Analysis of Locally Nonlinear Structures Using Substructure-Based State Equations (부분구조의 상태방정식을 이용한 국부 비선형계의 과도응답해석)

  • 김형근;박윤식
    • Proceedings of the Korean Society for Noise and Vibration Engineering Conference
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    • 1993.04a
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    • pp.52-56
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    • 1993
  • An efficient method is presented for determining transient responses of locally nonlinear structures using substructure eigenproperties and Lagrange multiplier technique. The method is based upon the mode synthesis formulation procedure, but does not construct the equations of motion of the combined whole structure compared with the conventional methods. For modal bases of each linear substructure, either fixed or free interface modes can be employed. The transient analysis is based upon the recurrence discrete-time state equations and offers the simplicity of the Euler integration method without requiring small time increment and iterative solution procedure. Numerical examples reveal that the method is very accurate and efficient in calculating transient responses compared with the direct numerical integration method.

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Antiinflammatory Evaluation and Synthesis of Benzothiazine Derivatives as Cyclooxygenase-2 Inhibitor (Cyclooxygenase-2 저해제로서의 benzothiazine 유도체 합성과 항염작용 평가)

  • 신혜순;박명숙;권순경
    • YAKHAK HOEJI
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    • v.44 no.3
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    • pp.272-278
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    • 2000
  • The antiinflammatory mechanism of NSAIDs is attributed to the reduction of prostaglandin synthesis by the direct inhibition of cyclooxygenase. Inhibition of prostaglandin production in organs such as stomach and kidney can result in gastric lesions, nephrotoxicity and increased bleeding. In this study, newly designed COX-2 inhibitors, synthesized 1,2-benzothiazine derivatives, were screened in vitro for selectivity of COX-1 and COX-2 inhibition properties. Lead compounds in the structure-activity relationship were studied to synthesize new highly selective COX-2 inhibitors.13 determine inhibitory effect of COX-2, synthesized 1,2-benzothiazine derivatives were screened with accumulation of prostaglandin by lipopolysaccharide (LPS) in aspirin-treated macrophages and murine macropharge cell. Some of synthesized 1,2-benzothiazine derivatives were shown to be effective as selective COX-2 inhibitory activity. Others exhibited a preferential inhibition of COX-2, although some COX-1 inhibitory activity was still present. As a conclusion, simple monomer derivatives were more active than dimer derivatives. Substitution of halogen (Br, C1) on the benzothiazine nucleus slightly enhanced inhibition activity.

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Substructure/fluid subdomain coupling method for large vibroacoustic problems

  • El Maani, Rabii;El Hami, Abdelkhalak;Radi, Bouchaib
    • Structural Engineering and Mechanics
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    • v.65 no.4
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    • pp.359-368
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    • 2018
  • Dynamic analysis of complex and large structures may be costly from a numerical point of view. For coupled vibroacoustic finite element models, the importance of reducing the size becomes obvious because the fluid degrees of freedom must be added to the structural ones. In this paper, a component mode synthesis method is proposed for large vibroacoustic interaction problems. This method couples fluid subdomains and dynamical substructuring of Craig and Bampton type. The acoustic formulation is written in terms of the velocity potential, which implies several advantages: coupled algebraic systems remain symmetric, and a potential formulation allows a direct extension of Craig and Bampton's method to acoustics. Those properties make the proposed method easy to implement in an existing finite element code because the local numerical treatment of substructures and fluid subdomains is undifferentiated. Test cases are then presented for axisymmetric geometries. Numerical results tend to prove the validity and the efficiency of the proposed method.

MEASUREMENT OF SYNTHESIS RATE OF LONG-CHAIN ACYL-COENZYME A ESTER IN BOVINE LIVER BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

  • Mitsuhashi, T.;Mitsumoto, M.;Yamashita, Y.;Ozawa, S.
    • Asian-Australasian Journal of Animal Sciences
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    • v.1 no.2
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    • pp.99-106
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    • 1988
  • A high performance liquid chromatographic procedure is described for the direct determination of the picomole amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A, using a stainless steel column packed with C-18 derivatized porous silica ($5{\mu}m$), an isocratic elution with a mixture of 33 mM $KH_2PO_4$/acetonitrile as a mobile phase and a UV detector. The long-chain acyl-Coenzyme A esters were determined in incubated microsomal fractions of a bovine liver to demonstrate the utility of this method for monitoring acyl-CoA synthesis in biological samples. The reaction rate of palmitate was higher than that of stearate. After a 60 minute incubation period, the generated amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A were approximately 70 and 20 n mol/mg micresomal protein, respectively. The advantage of this method are in that no decomposition of the CoA esters is involved, while the constituent molecular species is detected.

Design of Advanced Multi-loop PI Controller for Multi-delay Processes (다중 시간지연 공정을 위한 개선된 다중루프 PI 제어기 설계)

  • Vu, Truong Nguyen Luan;Lee, Moon-Yong
    • Journal of Institute of Control, Robotics and Systems
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    • v.16 no.1
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    • pp.77-82
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    • 2010
  • An analytical method for robust design of the multi-loop proportional-integral (PI) controller is proposed for various types of multi-delay processes. On the basis of the direct synthesis and generalized IMC-PID approach, the analytical tuning rules of the multi-loop PI controller are firstly derived for achieving the desired closed-loop response, and the structured singular value synthesis is then utilized for the tradeoffs between the robust stability and performance by adjusting only one design parameter (i.e., the closed-loop time constant). To verify the superiority of the proposed method, the simulation studies have been conducted on a wide variety of multivariable processes. The multi-loop PI controller designed by the proposed method shows a fast, well-balanced and robust response with the minimum integral absolute error (IAE) in compared with other renowned methods.

Systematic Design of High-Resolution High-Frequency Cascade Continuous-Time Sigma-Delta Modulators

  • Tortosa, Ramon;Castro-Lopez, Rafael;De La Rosa, J.M.;Roca, Elisenda;Rodriguez-Vazquez, Angel;Fernandez, F.V.
    • ETRI Journal
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    • v.30 no.4
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    • pp.535-545
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    • 2008
  • This paper introduces a systematic top-down and bottom-up design methodology to assist the designer in the implementation of continuous-time (CT) cascade sigma-delta (${\Sigma}{\Delta}$) modulators. The salient features of this methodology are (a) flexible behavioral modeling for optimum accuracy-efficiency trade-offs at different stages of the top-down synthesis process, (b) direct synthesis in the continuous-time domain for minimum circuit complexity and sensitivity, (c) mixed knowledge-based and optimization-based architectural exploration and specification transmission for enhanced circuit performance, and (d) use of Pareto-optimal fronts of building blocks to reduce re-design iterations. The applicability of this methodology will be illustrated via the design of a 12-bit 20 MHz CT ${\Sigma}{\Delta}$ modulator in a 1.2 V 130 nm CMOS technology.

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Synthesis of Silver Nanoplates with Fibronectin Nanofibril Template and Their SERS Applications

  • Wang, Li;Sun, Yujing;Cui, Yuncheng;Wang, Jiku;Li, Zhuang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.443-446
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    • 2013
  • In this work, a novel strategy is provided to prepare silver nanoplates by a fibronectin (Fn) nanofibril template. First, Fn molecules were controlled to assemble into amyloid-like nanofibrils in highly concentrated ethanol aqueous solution. The resultant nanofibrils could serve as a soft template to direct the formation of silver nanoplates. It is worth noting that the silver nanoplates are excellent surface-enhanced Raman scattering (SERS) substrate with 4-aminothiophenol (4-ATP) molecule as a test probe. This high active SERS substrate can also be used to detect drug molecule, 2-thiouracil with high sensitivity.