• Title/Summary/Keyword: NMR spectrometer

Search Result 103, Processing Time 0.035 seconds

Synthesis of $\pi$-Allyl-type Cobalt, Palladium, Platinum Complexes Having a $C_2$-Chiral Ligand ($C_2$ 손대칭 리간드를 배위하는 $\pi$-Allyl-Cobalt, Palladium, Platinum 착물의 생성)

  • Uhm, Jae Kook;Lee, Jong O;An, Hee Won
    • Journal of the Korean Chemical Society
    • /
    • v.42 no.2
    • /
    • pp.177-183
    • /
    • 1998
  • By the reactions of a $C_{2}$-chiral ligand, (+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene(6) with $[\pi-allyl chloroplatinum(II)]_4$, and $CpCo(CO)_2$ respectively, three new complexes, ($\pi$-allyl)platinum(II)(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene perchlorate(1), ($\pi$-allyl)platinum(II)(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene chloride(2), ($\eta^5$-cyclopentadienyl)cobalt(I)-(+)-11S,12S-bis[2,2'-(diphenylphosphino)benzanilido]-9,10-dihydro-9,10-ethanoanthracene(3) were prepared. $\eta^3$-Cyclohexenyl)palladium(II)1,2-bis(diphenylphosphino)ethane perchlorate(4) was obtained by the reaction of ($\eta^3$-cyclohexenyl)palladium(II) chloride dimer with a symmetric ligand, 1,2-bis(diphenylphosphino)ethane and lithium perchlorate. These complexes were identified by NMR-, IR-, and Mass-Spectrophotometers and elemental analyzer.

  • PDF

Synthesis and Properties of Liquid Crystal Compounds and Epoxy Resin Based Side Chain Liquid Crystal Polymers I. Low Molecular Weight Liquid Crystal Compounds (방향족 액정동족체 및 Epoxy형 측쇄 액정고분자의 합성 및 성질 I. 저분자 액정 동족체)

  • Park, Se Kwang;Ahn, Wonsool;Keum, Chang Dae;Park, Lee Soon
    • Applied Chemistry for Engineering
    • /
    • v.9 no.1
    • /
    • pp.66-70
    • /
    • 1998
  • Several liquid crystalline monomers were synthesized and characterized to utilize as new matrix materials of liquid crystal/polymer composite films for display application. Liquid crystalline compounds which have azo group as center link, cyano group at one of the terminal position in common and bromoalkyl(azo(n)), azidoalkyl(AZI(n)), aminoalkyl(ALC(n)) as the terminal group were synthesized and identified respectively by FT-lR, $^1H-NMR$ spectrometer and elemental analysis. All these compounds exhibited nematic liquid crystalline region in the certain temperature range as determined by DSC and polarized optical microscope. These liquid crystalline compounds also showed a typical even-odd effect in both $T_{KN}$ and $T_{NI}$ due to conformational change as the length of terminal alkyl chain, $-(CH_2)n-$. was varied.

  • PDF

Synthesis and Physical Properties of Polycaprolactone Based Polyurethanes Using Aliphatic or Aromatic Diisocyanates (지방족 및 방향족 이소시아네이트를 이용한 폴리카프로락톤계 폴리우레탄의 합성 및 물성 연구)

  • Kim Sun-Mi;Kwak Noh-Seok;Yang Yun-Kyu;Yim Bong-Kyun;Park Bo-Young;Hwang Taek-Sung
    • Polymer(Korea)
    • /
    • v.29 no.3
    • /
    • pp.253-259
    • /
    • 2005
  • Polyurethanes, synthesized by polyester polyols and aliphatic or aromatic diisocyanates for a crease resist finishing agent, were prepared by two-step reactions, that is, prepolymer synthesis and chain extension. The structures of synthesized polyurethanes were confirmed by the measurement of FT-IR and $^1H$-NMR spectrometer. The number average molecular weight ($\bar{M}_n$) and the weight average molecular weight ($\bar{M}_w$) of the polyurethane with aromatic diisocyanate (MDI) were higher than those of the synthesized polyurethanes with aliphatic diisocyanate (HDI, $H_{12}MDI$). The glass transition temperatures ($T_g$) of soft segments in polyurethanes with MDI, HDI, $H_{12}MDI$ were -25,-42 and -50$^{circ}C$, respectively. In the polyurethanes obtained by two-step reaction, thermal stability and tensile strength increased with increasing hard segment contents, whereas elongation at break decreased with increasing hard segment contents.

Fusion anti-cancer drugs of cisplatin analogue and fatty acids for multi-targeted cancer treatment (시스플라틴과 지방산을 결합한 퓨전 항암제)

  • Byeon, Hong-Ju;Lee, Hyang-Yeol
    • Journal of the Korean Applied Science and Technology
    • /
    • v.35 no.4
    • /
    • pp.1386-1392
    • /
    • 2018
  • Cispatin has become one of the most widely used anticancer drugs for decades. One of the drawback of cisplatin (II) complex is that it not only targets cancerous cells but also normal cells causing several serious side effects in patients. We have synthesized Pt(IV) complex that are needed to have the ability to kill target cells selectively in a short time before drug resistance develops. By introducing PDK inhibitor, butyric acid and valproic acid, on Pt complex, two fusion anti-cancer agents 3 and 4 have been synthesized and characterized their structures by nmr and mass spectrometer. MTT assay was performed with $Pt(IV)-Bu_2$ 3 and $Pt(IV)-Val_2$ 4 against MCF-7 cell line. As a result, cisplatin, Pt(IV) complexes 3 and 4 were treated, cell viabilities at $50{\mu}M$ cencentration were decreased to 39%, 54% and 84% respectively.

The study of chemical substances in Hymenoxys brachyactis(II) (Hymenoxys brachyactis의 화학성분에 관한 연구(II))

  • Lee, Sang-Jun;Kim, Sung-Han;Kim, Jung-Han
    • Applied Biological Chemistry
    • /
    • v.38 no.5
    • /
    • pp.473-477
    • /
    • 1995
  • The dichloromethane extracts of the above ground parts of Hymenoxys brachyactis afforded three sesquiterpene lactones already reported, one new sesquiterpene lactone, biennin C and hispidulin as known toxic flavone. Structures of all compounds were established by spectroscopy and biennin C was determined as an adduct of the modified pseudoguanolide and hymenoxon by Gas Chromatograpy and MS spectrometer These sesquiterpene lactones have the same ${\alpha},{\beta}$-unsaturated functional group like that of hymenovin which has been known as major toxic constituent of important livestock poison. And biennin C is also considered as toxic compound because of toxic hymenoxon.

  • PDF

The Inhibitory Constituents from the Ginger on a Drug Metabolizing Enzyme CYP3A4 (생강의 약물대사효소 CYP3A4 저해 성분)

  • 차배천;이은희;권준택
    • YAKHAK HOEJI
    • /
    • v.48 no.5
    • /
    • pp.266-271
    • /
    • 2004
  • Ginger (Zingiber officinale Roscoe) is widely used as a common condiment for a variety of foods and beverages. In addition to its extensive utilization as a spice, the fresh or the processed rhizome is a useful crude drug in traditional Chinese medicine. It is considered to possess stomachic, carminative, stimulant, diuretic and antiemetic properties. Chemical studies on the pungent principles of ginger have been carried out by a number of investigators, and 6-gingerol and 6-shogaol as a major pungent substance have been isolated. In this study, the constituents inhibiting a drug metabolizing enzyme CYP3A4 from ginger were investigated. CYP3A4 is responsible for drug metabolism as heme-containing monooxygenases. As a result of experiment, 10-gingerol (lC$_{50}$ 5.75$\mu$M) isolated from EtOAc extract of ginger showed remarkable inhibitory activity compared to 6-gingerol ($IC_{50}$/ 14.56 $\mu$M) and zingerone ($IC_{50}$/ 379.63 $\mu$M). This paper describes the isolation, structure elucidation, and CYP3A4 inhibitory activity of these compounds. The structure of the compounds were identified by instrumental analysis such as LC-mass spectrometer and NMR.R.

Studies on the Reactions of Urea with Paraformaldehyde (Urea와 Paraformaldehyde 반응산물(反應産物)의 화학적(化學的) 특성(特性) 연구)

  • Choi, Du-Hoi;Norwood, Verrill M.
    • Korean Journal of Soil Science and Fertilizer
    • /
    • v.24 no.1
    • /
    • pp.41-49
    • /
    • 1991
  • The reaction of molten urea with paraformaldehyde in sealed tubes has been examined, and the concentrations of the products obtained from this reaction have been contrasted to previous results from the identical reaction carried out in open beakers. In these studies, high performance liquid chromatography(HPLC) and nuclear magnetic resonance(NMR) spectroscopy were used to analyze the products formed in the reactions. These products were biuret, triuret, dimethylenetriurea, methylenediurea, and biuretmethyleneurea. The results from the HPLC analyses showed that the concentrations of dimethylenetriurea and methylenediurea in the reaction products increased as the amount of the paraformaldehyde starting material increased. However, the amount of biuret formed in the products decreased as the paraformaldehyde concentration was increased in the urea melt. The results from the NMR analyses showed that the $NH_2$ resonance frequencies for urea, methylenediurea, and dimethylenetriurea all occurred at approximately 5.6 ppm, while the $NH_2$ frequencies for biuret and triuret occurred at approximately 6.9ppm. In the case of biuret and triuret, NH protons absorb between 8.5 and 9.5 ppm, whereas the NH protons in methylenediurea and dimethylenetriurea absorb in the 6.5-6.6ppm region. The melt reaction seems to hold promise as a different technique for ureaform preparation in general.

  • PDF

Discrimination model of cultivation area of Corni Fructus using a GC-MS-Based metabolomics approach (GC-MS 기반 대사체학 기법을 이용한 산수유의 산지판별모델)

  • Leem, Jae-Yoon
    • Analytical Science and Technology
    • /
    • v.29 no.1
    • /
    • pp.1-9
    • /
    • 2016
  • It is believed that traditional Korean medicines can be managed more scientifically through the development of logical criteria to verify their region of cultivation, and that this could contribute to the advancement of the traditional herbal medicine industry. This study attempted to determine such criteria for Sansuyu. The volatile compounds were obtained from 20 samples of domestic Corni fructus (Sansuyu) and 45 samples of Chinese Sansuyu by steam distillation. The metabolites were identified in the NIST Mass Spectral Library via the obtained gas chromatography/mass spectrometer (GC/MS) data of 53 training samples. Data binning at 0.2 min intervals was performed to normalize the number of variables used in the statistical analysis. Multivariate statistical analyses, such as principle component analysis (PCA), partial least squares-discriminant analysis (PLS-DA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) were performed using the SIMCA-P software package. Significant variables with a variable importance in the projection (VIP) score higher than 1.0 were obtained from OPLS-DA, and variables that resulted in a p-value of less than 0.05 through one-way ANOVA were selected to verify the marker compounds. Finally, among the 11 variables extracted, 1-ethylbutyl-hydroperoxide (9.089 min), nonadecane (20.170 min), butylated hydroxytoluene (25.319 min), 5β,7βH,10α-eudesm-11-en-1α-ol (25.921 min), 7,9-bis(2-methyl-2-propanyl)-1-oxaspiro[4.5]deca-6,9-diene-2,8-dione (34.257 min), and 2-decyldodecyl-benzene (54.717 min) were selected as markers to indicate the origin of Sansuyu. The statistical model developed was suitable for the determination of the geographical origin of Sansuyu. The cultivation areas of four Korean and eight Chinese Sansuyu samples were predicted via the established OPLS-DA model, and it was confirmed that 11 of the 12 samples were accurately classified.

A Synthesis of Alkylphenyl fluorobenzoate Derivatives and Their Antifungal Activities on Several Phytopathogens (Alkylphenyl fluorobenzoate 유도체들의 합성과 몇 가지 식물병원균에 대한 항균활성)

  • Choi, Won-Sik;Cha, Kyung-Min;Kim, Young-Sun;Jang, Soon-Ho;Lim, Sang-Ho;Choi, In-Young;Kim, Tae-Jun;Jung, Bong-Jin
    • The Korean Journal of Pesticide Science
    • /
    • v.12 no.4
    • /
    • pp.307-314
    • /
    • 2008
  • Sixty compounds such as alkylphenyl fluorobenzoate esters from thymol(I), 5-isopropyl-3-methylphenol (II), 4-isopropyl-3-methylphenol (III), 2-sec-butylphenol (IV) and 4-sec-butylphenol (V) were synthesized. These derivatives were identified by IR, $^1H$-NMR spectrometer and GC/MS. Their in vivo antifungal activities were tested against phytopathogens such as Phytophthora infestans, Botrytis cinerea, Colletotrichum orbiculare and Rhizoctonia solani. As the result, 2-sec-butylphenyl 2,5-difluorobenzoate (IV-6) and 4-sec-butylphenyl 2,5-difluorobenzoate (V-6) showed 90% above antifungal activity against Botrytis cinerea. 2-Isopropyl-5-methylphenyl 2,3,6-trifluorobenzoate (I-11), 2-isopropyl-5-methylphenyl 2,4,5-trifluorobenzoate (I-12), 5-isopropyl-3-methylphenyl 2,3,6-trifluorobenzoate (II-11), 4-isopropyl-3-methylphenyl 2,3,6-trifluorobenzoate (III-11) and 4-isopropyl-3-methylphenyl 2,4,5-trifluorobenzoate (III -12) showed 90% above potent antifungal activity against Colletotrichum orbiculare.

Polymeric Micelle Using Poly((R)-3-hydroxybutyric acid)/Poly(ethylene glycol) Amphiphilic Block Copolymer for Drug Delivery System (Poly((R)-3-hydroxybutyric acid)/Poly(ethylene glycol) 양친성 블록 공중합체를 이용한 약물전달체용 고분자 미셀)

  • Jeong, Kwan-Ho;Kim, Young-Jin
    • Polymer(Korea)
    • /
    • v.30 no.6
    • /
    • pp.512-518
    • /
    • 2006
  • A biodegradable polymer poly((R) -3-hydroxybutyric acid) (PHB) was conjugated with a hydrophilic polymer poly(ethylene glycol) (PEG) by the ttansesterification reaction to form the amphiphilic block copolymer. PHB with low molecular weight ($3000{\sim}30000$) was appropriated for the drug delivery materials. High molecular weight PHB was hydrolyzed by an acid-catalyst to produce the low molecular weight one. Amphiphilic block copolymer was formed the self-assembled polymeric micelle system in the aqueous solution that the hydrophillic PEG was wraped the hydrophobic PHB. Generally, polymeric micelle forms the small particle between $10{\sim}200nm$. These polymeric micelle systems have been widely used for the drug delivery systems because they were biodegradable, biocompatible, non-toxic and patient compliant. The hydroxyl group of PEG was substituted with carboxyl group which has the reactivity to the ester group of PHB. Amphiphilic block copolymer was conjugated between PHB, and modified PEG at $176^{\circ}C$ which was higher than the melting point of PHB. Transesterification reaction was verified with DSC, FTIR, $^1H-NMR$. In the aqueous solution, critical micelle concentration (CMC) of the mPEG-co-PHB copolymer measured by the fluororescence scanning spectrometer was $5{\times}10^{-5}g/L$. The shape and size of the nanoparticle was taken by dynamic light scattering and atomic force microscopy. The size of the nanoparticle was about 130 nm and the shape was spherical. Our polymeric micelle system can be used as the passive targeting drug delivery system.