• 제목/요약/키워드: IR and $^1H$ NMR spectra

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Synthesis, spectral, thermal, structural study and theoretical treatment of new complexes of mannich base with Ni(II) and study of cytotoxicity effect on (Hepa-2) cell line and antimicrobial activity

  • Omar H. Al-Obaidi
    • 분석과학
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    • 제36권2호
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    • pp.70-79
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    • 2023
  • The synthesis of the Mannich base as a ligand (L) N-(morpholino (phenyl) methyl) acetamide is the subject of this study. Elemental analyses, FT-IR spectra, UV-vis, 1H-NMR, and magnetic measurements were used to confirm the synthesis of the [Ni(L)2]Cl2 complex, thermal analysis (TG/DTG), atomic absorption, and scanning, and structurally explained as electron microscopy (SEM), and X-ray powder diffraction (XRD) methods. The melting point of the complex and its molar conductivity were also measured. The suggested geometries of the complexes formed have a tetrahedral structure, according to the data acquired using various techniques. Theoretical approaches to the complex formation have been investigated. For molecular mechanics and semi-empirical calculations, the HYPERCHEM6 program had been used. The effect of the novel Ni(II) complex on the cancer cell Hepa-2 (human hepatocellular ademocarcinoma), that is the human laryngeal cancer, was studied. It has been found that these ligand and complex have potent effects on the cancer cell. The antibacterial activity of the free ligand and its complex was evaluated against two kinds of human pathogenic bacteria. The first category is Gram-positive (Staphylococcus aureas, epiderimids), whereas the second group is Gram-negative (Psedamonas aeruginosa, Escherichia coli) (from the diffusion method). Finally, it was discovered that various chemicals had varied growth-inhibiting effects on bacteria.

Synthesis and Antitumor Activity of Phthalimide-Based Polymers Containing Camptothecin

  • Lee, Neung-Ju
    • Macromolecular Research
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    • 제11권1호
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    • pp.47-52
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    • 2003
  • The objective of this study was to develop a polymeric drug delivery system for camptothecin (CPT), capable of improving its therapeutic index and reducing its side effects. A monomeric conjugate, 3,6-endo-methylene-1,2,3,6-tetrahydrophthalimidoethanoylcamptothecin in (ETECPT) between CPT and 3,6-endo-methylene-1,2,3,6-tetrahydrophthalimidoethanoic acid was synthesized. Its homo-and copolymer with acrylic acid (AA) were prepared by photopolymerization using 2,2-dimethoxy-2-phenylacetophenone (DMP) as a photoinitiator. The monomer and its polymers were characterized by IR, $^1$H- and $^{13}$ C-NMR spectra. The ETECPT content in poly(ETECPT-co-AA) obtained by elemental analysis was 82 wt%. The number-average molecular weights of the polymers determined by gel permeation chromatography were as follows: M$_{n}$ = 11,400 for poly(ETECPT), M$_{n}$ = 17,900 for poly(ETECPT-co-AA). The $IC_{50}$/ values of ETECPT and its polymers against cancer cells were much larger than that of CPT. Our results from the in vivo antitumor activity indicated that all polymers show high antitumor activity than CPT at a dose of 100 mg/kg./kg.

오징어(Omnastrephes bartrami) 간지질(肝脂質)에 존재(存在)하는 Ethyl Acylates의 구조(構造)와 그 구성(構成) 지방산(脂肪酸) 조성(組成)에 관한 연구(硏究) (The Presence of Ethyl Acylates in the Liver Lipids of A Squid, Omnastrephes bartrami and Their Fatty Acid Composition)

  • 조연주;조용계
    • 한국응용과학기술학회지
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    • 제7권2호
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    • pp.19-32
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    • 1990
  • Lipid levels in the tissues of liver and intestines of O.bartrami amounted to 40.0% and 1.5%. The new compounds was found to be ethyl acylates, from a deduction of their detailed $^1H-nuclear$ magnetic resonance(NMR) and $^{13}C-NMR$ as well as infra red spectra (IR). The fatty acid composition of total lipids were mainly composed of C16:0(19.0%), C18:1(16.2%) and $C22:6{\omega}3$(15.7%), followed by C20:1(9.4%), C22:1(6.4%) and C18:0(5.4%). New compound A and B were seemed to derived from the cleavage of glycerol moieties of triglycerides by microbial activities during storage in a frozen state. Compound A contained C16:0(38.2%), C18:1(13:4%), C20:1(13.3%) and C22:1(11.7%) as major components, while compound B predominantly comprised polyunsaturated fatty acid such as $C20:5{\omega}3$ (41.2%) and $C22:6{\omega}3$(36.1%). In both compounds small amounts of odd numbered fatty acids were also detected ($3.8{\sim}2.2%$).

벤조사이오펜을 기초로 한 새로운 비대칭형 올리고머의 합성과 OTFT 특성 (Synthesis of Novel Asymmetric Oligomers Based on Benzothiophene and OTFT Characteristics)

  • 이동희;박종원;정대성;박찬;김윤희;권순기
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2010년도 하계학술대회 논문집
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    • pp.129-129
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    • 2010
  • The conjugated oligomers with rigid and fused-ring structures are of interest for the solution-processable organic thin film transistors (OTFTs) due to their well defined structure and high purity. In this study, alkyl substituted benzothiophene based oligomers were synthesized by a novel route, the key point of which is the acid-induced intermolecular cyclization reaction of aromatic methyl sulfoxides, and were confirmed by $^1H$-NMR and FT-IR studies. The obtained oligomers showed the good solubility in common organic solvents such as hexane, chloroform, and dimethylchloride at room-temperature, which is due to the introduced alkyl chain. The physical and optical properties of the oligomers were studied using differential scanning scalorimetry (DSC), cyclic-voltammetry (CV), UV-visible and PL spectra studies. Solution processed OTFT device based on synthesized oligomers show a high hole mobility of up to $0.01\;cm^2V^{-1}s^{-1}$, $I_{on}/I_{off}$ of $10^5$ and threshold voltage of -14V.

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친환경 접착제 제조용 아크릴계 반응성 유화제의 합성 (Synthesis and Charaterization of Polymerizable Acryl's Emulsifier to prepare Green Glue)

  • 정노희;박종권;강윤석
    • 한국응용과학기술학회지
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    • 제33권1호
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    • pp.51-57
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    • 2016
  • 이 연구에서는 계면활성제에 작용기를 첨가하여 유화제 뿐만 아니라 합성에서의 모노머로 작용할 수 있는 반응성 계면활성제를 합성하였다. 반응성 계면 활성제는 메타아크릴 산, 아크릴산과 비이온성 계면 활성제인 폴리 옥시 에틸렌 라우릴 에테르 (POE 23)를 사용하여 합성되었으며 벤젠을 용매로서 사용하였고, P-TsOH를 촉매로서 사용 하였다. 합성된 계면 활성제는 FT-IR, $^1H$-NMR 스펙트럼, 원소 분석을 하였다. 물성 평가는 HLB, Cloud point, 표면 장력, 임계 미셀 농도를 측정 하였다. HLB 값은 11.62~12.09 범위로 평가 하였다. cmc 값은 표면 장력 법으로 측정하였을 때 $1{\times}10^{-4}{\sim}5{\times}10^{-4}$의 값을 가졌다. 실험을 통해 측정된 Cloud point은 35, $39^{\circ}C$ 이었다. 합성 계면 활성제의 유화 특성은 polyoxyethylene lauryl ether보다 낮았다. 또한, 유화력은 벤젠에서 보다 대두유에서 더 좋았다. 실험결과 합성 수율은 93.27 ~ 94.49%로 확인되었다.

EO, PO가 부가된 도데실 에테르 황산화물의 합성 (Synthesis of Dodecyl Ether Sulfates Containing Various Ethylene Oxide and Isopropylene Oxide)

  • 유영창;노승호;주명종;남기대
    • 공업화학
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    • 제7권2호
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    • pp.289-298
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    • 1996
  • Dodecanol에 ethylene oxide(EO)와 isopropylene oxide(PO)를 각각 5, 10몰 씩 부가하고, EO 부가물에는 PO를 PO 부가물에는 EO를 또 다시 5, 10몰 씩 부가시킨 다음 클로로술폰산으로 황산화시켜 8종의 음이온계면활성제를 합성하였다. 8종의 sodium poly(oxyethylene, oxyisopropylene) dodecyl ether sulfate에 대한 EO 및 PO의 부가를 확인하기 위하여 고성능액체크로마토그래피, 프로톤핵자기공명스펙트럼, 히드록시기값, 적외선스펙트럼을 사용하였다. 그리고 황산화를 확인하기 위하여 스펙트라와 Epton법을 이용하여 EO 및 PO 분자수를 확인하였다. 이 결과 황산화 반응의 최종 생성물의 수율은 90~96%로써 비교적 높게 얻을 수 있었다.

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Synthesis of a Novel Phosphorus-containing Flame Retardant for Epoxy Resins

  • Xu, Hong-Jun;Jin, Fan-Long;Park, Soo-Jin
    • Bulletin of the Korean Chemical Society
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    • 제30권11호
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    • pp.2643-2646
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    • 2009
  • In this study, a novel phosphorus-containing flame retardant copolymer of spirocyclic pentaerythritol di(phosphate monochloride) and bisphenol S (SPD-BS) was successfully synthesized and used as a flame retardant in diglycidyl ether of bisphenol A (DGEBA) epoxy resins. The chemical structure of the SPD-BS was characterized using FT-IR and $^1H$ NMR spectra. The thermal properties were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The effects of SPD-BS and nano-$CaCO_3$ on the flame-retardant properties of DGEBA/SPD-BS systems were evaluated by measurement of the burning rate. As a result, the thermal stabilities of the DGEBA/SPD-BS systems were decreased with increasing SPD-BS content. The flame-retardant properties and char yields of the systems were significantly increased when SPD-BS content increased. The synergism of nano-$CaCO_3$ incorporation on flame retardancy was found for the DGEBA/SPD-BS systems.

Thymol과 Carvacrol 유도체들의 합성과 식물병원균에 대한 항균활성 (In vitro and in vivo antifunal activaties of derivatives of thymol( I ) and carvacrol(II) againt phytopathogenic fungi)

  • 최원식;정찬진;장도연;차경민;엄대용;김태준;정봉진
    • 농약과학회지
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    • 제10권4호
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    • pp.237-248
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    • 2006
  • 항균활성을 나타내는 thyme oil의 주성분인 thymol(I)과 carvacrol(II)을 출발물질로 하여 ester, sulfonyl ester, carbamate, ether와 phosphoyl ester 계열 유도체 41종을 합성하였다. IR, GC/MS 와 $^1H$-NMR spectrum을 이용하여 합성된 화합물들을 확인하였다. 이들 유도체들을 10종의 식물 병원균에 대하여 항균활성 실험을 실시한 결과 몇가지 화합물이 우수한 항균활성을 나타내었다. 이들 화합물에 대한 in vivo실험은 오이, 토마토와 벼 작물에서 실시하였다. 그 결과, 2-isopropyl-5-methylphenyl acetate(I-1a)가 오이 잿빛곰팡이 병균(Botrytis cinerea)과 벼도열병균(Pyrcularia oryzae)에 높은 항균활성을 나타내었으며, methyl(2-isopropyl-5-methylphenoxy)acetate(I-6d)는 벼 잎집무늬마름병균(Rhizoctonia solani)에서 ethyl4-(2-methyl5-isopropylphenoxy)-crotonate(I-7d)는 토마토역병균(Phytophthora infestans)에서 우수한 항균활성을 나타내었다.

벼(Oryza sativa L.)의 지상부로부터 adenosine과 phlomuroside의 분리 및 동정 (Isolation and Identification of Adenosine and Phlomuroside from the Aerial Parts of Oryza sativa L.)

  • 정락훈;이대영;조진경;백윤수;서경화;이동걸;강희철;김지영;백남인
    • Journal of Applied Biological Chemistry
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    • 제57권4호
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    • pp.321-324
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    • 2014
  • 벼 지상부를 MeOH 수용액으로 추출하고 이 추출물을 n-hexane, EtOAc, n-BuOH, 및 $H_2O$ 분획으로 나누었다. n-BuOH 분획에 대하여 silica gel, ODS 및 Sephadex LH-20 column chromatography를 반복실시 하여 2종의 화합물을 분리하였다. NMR, IR 및 MS data를 해석하여 각각 adenosine (1)과 phlomuroside (2)로 구조 동정 하였다. 이들 화합물들은 벼에서는 처음으로 분리되었다.

Chemoenzymatic Synthesis of Dual-responsive Amphiphilic Block Copolymers and Drug Release Studies

  • Chen, Peng;Li, Ya-Peng;Wang, Shu-Wei;Meng, Xin-Lei;Zhu, Ming;Wang, Jing-Yuan
    • Bulletin of the Korean Chemical Society
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    • 제34권6호
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    • pp.1800-1808
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    • 2013
  • Dual-responsive amphiphilic block copolymers were synthesized by combining enzymatic ring-opening polymerization (eROP) of ${\varepsilon}$-caprolactone (CL) and ATRP of N,N-dimethylamino-2-ethyl methacrylate (DMAEMA). The obtained block copolymers were characterized by gel permeation chromatography (GPC), $^1H$ NMR and FTIR-IR. The critical micelle concentration (CMC) of copolymer was determined by fluorescence spectra, it can be found that with hydrophilic block (PDMAEMA) increasing, CMC value of the polymer sample increased accordingly, and the CMC value was 0.012 mg/mL, 0.025 mg/mL and 0.037 mg/mL for $PCL_{50}$-b-$PDMAEMA_{68}$, $PCL_{50}$-b-$PDMAEMA_{89}$, $PCL_{50}$-b-$PDMAEMA_{112}$, $PCL_{50}$-b-$PDMAEMA_{89}$ was chosen as drug carrier to study in vitro release profile of anti-cancer drug (taxol). The temperature and pH dependence of the values of hydrodynamic diameter (Dh) of micelles, and self-assembly of the resulting block copolymers in water were evaluated by dynamic light scattering (DLS). The result showed that with the temperature increasing and pH decreasing, the Dh decreased. Drug-loaded nanoparticles were fabricated using paclitaxel as model. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) had been explored to study the morphology of the hollow micelles and the nanoparticles, revealing well-dispersed spheres with the average diameters both around 80 nm. In vitro release kinetics of paclitaxel from the nanoparticles was also investigated in different conditions (pH and temperature, etc.), revealing that the drug release was triggered by temperature changes upon the lower critical solution temperature (LCST) at pH 7.4, and at $37^{\circ}C$ by an increase of pH.