• Title/Summary/Keyword: Bis(pyridine)

Search Result 64, Processing Time 0.032 seconds

Methylation Methods on Identification of Phenolics in Chebulae Fructus (Chebulae Fructus중 페놀 물질 확인시의 Methylation법 비교)

  • 김정숙
    • Journal of the East Asian Society of Dietary Life
    • /
    • v.4 no.1
    • /
    • pp.79-86
    • /
    • 1994
  • Food quality in food processing and storage were affected by the kinds of phenolics involved. To analyze phenolics of Chebulae Fructus by the way of GC-MSm methylation and trimethylsilyation(TMS) are necessary. The methods of methylation were dimethyl sulfate method and diazomethane method. so this study was undertaken to research the better methylation method before measuring GC-MS. But dimethyl sulfate method of methylation was not sufficient to analyze phenolics. So the phenolics of Chebulae Fructus were analyzed by the diazomethane methylation method and TMS with the pyridine, N-O-bis-trimethylsilyl-acetamide(BSTFA) and trimethylchlorosilane(TMCS). With the exception of pyrogallol and phloroglucinol in insoluble phenolics of Chebulae Fructus, the greater part of phenolics. analysis could be analyzed by GC-MS in company with diazomethane methylation method and TMS.

  • PDF

Synthesis of Rosinimide Modified with Polyphenylpyridinylsiloxane and Its Characteristics

  • Kang, Doo-Whan;Kim, Young-Min
    • Fibers and Polymers
    • /
    • v.1 no.2
    • /
    • pp.67-70
    • /
    • 2000
  • Rosin maleic anhydride adduct (RMA)-bisester was prepared by the esterification of chlorinated RMA with hydroquinone. Phenylpyridinylcyclot.isiloxane ($D_3^{Ph,Py}$) was synthesized from phenylpyridinyldichlorosilane in the presence of zinc oxide catalyst, and amino group terminated polyphenylpyridinylsiloxane prepolymer was prepared by equilibrium polymerization of $D_3^{Ph,Py}$ with 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane. Rosinimide (PSMR) was prepared from the imidization of RMA-bisester with polyphenylpyridinylsiloxane prepolymer at 12$0^{\circ}C$ for 7 h using ${\gamma}$-butyrolactone/pyridine. It showed that PSMR had better thermal stalbility than rosinimide modified with polydimethylsiloxane.

  • PDF

Synthesis and Characterization of Fluorinated Polybenzoxazole Copolymers

  • Sohn, Jeong Sun;Park, A Ram;Choi, Jae Kon
    • Elastomers and Composites
    • /
    • v.50 no.3
    • /
    • pp.175-183
    • /
    • 2015
  • A series of fluorinated aromatic poly(hydroxyamide)s (PHAs) were synthesized by direct polycondensation of diacides containing 2,6-dimethylphenoxy group and quinoxaline ring in the main chain with 2,2-bis-(3-amino-4-hydroxyphenyl) hexafluoropropane. The PHAs had relatively low inherent viscosities in the range of 0.35~0.43 dL/g at $35^{\circ}C$ in DMAc solution. All PHAs exhibited excellent solubility in aprotic solvents such as NMP, DMAc, DMF and DMSO as well as in common organic solvents such as pyridine, THF, and m-cresol at room temperature. However, the poly(benzoxazole)s (PBOs) were quite insoluble in all organic solvents except partially soluble in concentrated sulfuric acid. The PBOs showed glass transition temperatures between 233 and $284^{\circ}C$ by DSC and maximum weight loss temperatures in the range of $536-546^{\circ}C$ by TGA.

Crystal Structure and Characterization of a New Eight Coordinated Cadmium Complex

  • Hakimi, Mohammad;Moeini, Keyvan;Mardani, Zahra;Khorrami, Farzaneh
    • Journal of the Korean Chemical Society
    • /
    • v.57 no.3
    • /
    • pp.352-356
    • /
    • 2013
  • In this work, a new cadmium complex $[Cd(L)(CH_3COO)_2].2H_2O$ (1) with the ligand L, N,N'-bis(2-pyridinecarboxalidene)-1,2-cyclohexanediamine was prepared and identified by elemental analysis, FT-IR, Raman, $^1H$ NMR spectroscopy and single-crystal X-ray diffraction. The cadmium atom in the crystal structure of 1 has distorted triangular dodecahedral geometry by coordination of the four nitrogen atoms of L and four oxygen atoms of the two acetate ions. Two water molecules are also incorporated in the crystal network. The $O-H{\cdots}O$ hydrogen bonds present in the crystal structure of 1. In this work, three structural surveys including coordination numbers of the cadmium atom, coordination modes of L and resonance in pyridine-2-ylmethanimine-based compounds are presented.

Indentification of Some Metabolites of Carbinoxamine in Rat Urine (흰쥐 뇨에서의 Carbinoxamine의 대사체 확인)

  • 정병화;이선화;김태욱;정봉철;박종세
    • YAKHAK HOEJI
    • /
    • v.37 no.4
    • /
    • pp.317-324
    • /
    • 1993
  • The metabolic profile of carbinoxamine, 2-[(4-chlorophenyl)-2-pyridinyi-methoxy] N, N-dimethylethanamine, was determined in rat urine. Urinary extracts obtained with or without enzyme hydrolysis were derivatized with MSTFA/TMSCI (N-methyl-N-trimethylsilyl trifluoroacetamide/Trimethylchlorosilane) and analyzed by GC/MSD. In rat urine, which obtained after oral treatment with carbinoxamine maleate, chlorobenzolyl pyridine, (4-chlorophenyl)-2-pyridinyl methanol : carbinol, 2-[(4-chlorophenyl)-2-pyridinylmethoxy]-N-methylethanamine : norcarbinoxamine, 2-[(4-chlorophenyl)2-pyridinylmethoxy]ethanamine : bis-norcarbinoxamine and parent carbinoxamine were detected in free form. Norcarbinoxamine and bisnorcarbinoxamine were also detected in conjugated form(acetylation). These data suggest that in the rat, hydroxylation of either the benzyl or pyridinyl ring can occur during carbinoxamine elimination. O-demethylation and subsequent conjugation represents the primary pathway of carbinoxamine elimination in the rat.

  • PDF

1H NMR Study of Aziridine Derivatives Coordinated to the Paramagnetic Undecatungstocobalto(II)silicate and -nickelo(II)silicate Anions

  • 박석민;서현수
    • Bulletin of the Korean Chemical Society
    • /
    • v.18 no.9
    • /
    • pp.1002-1006
    • /
    • 1997
  • 1H NMR spectra of D2O solutions containing 2,2-dimethylaziridine (1) or 2-methylaziridine (2) and [SiW11COⅡO39]6- (SiW11Co) or [SiW11NiⅡO39]6- (SiW11Ni) exhibit separate signals for the free ligand and the complex, indicating that the ligand exchange is slow on the NMR time scale. Identified are two linkage isomers with the methyl group of 2 at trans or cis position with respect to the metal. The isotropic shifts of 1 and 2 coordinated to SiW11Ni originate mainly from the contact shifts, and they agree reasonably with the relative values reported for similar ligands coordinated to bis(2,4-pentanedionato)nickel(Ⅱ). The isotropic shifts for the SiW11Co complexes were separated into contact and pseudocontact contributions. The pseudocontact shifts show that (χ∥-χ⊥) is positive, while that for the SiW11Co complexes of pyridine derivatives is negative. This result indicates that the ordering of dxy and dxz, dyz orbitals in SiW11Co complexes can be reversed by ligands.

Three Cyanide-Bridged One-Dimensional Single Chain CoIII-MnII Complexes: Rational Design, Synthesis, Crystal Structures and Magnetic Properties

  • Zhang, Daopeng;Zhao, Zengdian;Wang, Ping;Chen, Xia
    • Bulletin of the Korean Chemical Society
    • /
    • v.33 no.5
    • /
    • pp.1581-1585
    • /
    • 2012
  • Two pyridinecarboxamide dicyanidecobalt(III) building blocks and two mononuclear seven-coordinated macrocycle manganese(II) compounds have been rationally selected to assemble cyanide-bridged heterobimetallic complexes, resulting in three cyanide-bridged $Co^{III}-Mn^{II}$ complexes. Single X-ray diffraction analysis show that these complexes $\{[Mn(L^1)][Co(bpb)]\}ClO_4{\cdot}CH_3OH{\cdot}0.5H_2O$ ($\mathbf{1}$), $\{[Mn(L^2)][Co(bpb)]\}ClO_4{\cdot}0.5CH_3OH$ ($\mathbf{2}$) and ${[Mn(L^1)][Co(bpb)]\}ClO_4{\cdot}H_2O$ ($\mathbf{3}$) ($L^1$ = 3,6-diazaoctane-1,8-diamine, $L^2$ = 3,6-dioxaoctano-1,8-diamine; $bpb2^{2-}$ = 1,2-bis(pyridine-2-carboxamido)benzenate, $bpmb2^{2-}$ = 1,2-bis(pyridine-2-carboxamido)-4-methyl-benzenate) all present predictable one-dimensional single chain structures. The molecular structures of these one-dimensional complexes consists of alternating units of $[Mn(L)]^{2+}$ ($L=L^1$ or $L^2$) and $[Co(L^{\prime})(CN)2]^-$ ($L^{\prime}=bpb2^{2-}$, or $bpmb2^{2-}$), forming a cyanide-bridged cationic polymeric chain with free $ClO_4{^-}$ as the balance anion. The coordination geometry of manganese(II) ion in the three one-dimensional complexes is a slightly distorted pentagonal-bipyrimidal with two cyanide nitrogen atoms at the trans positions and $N_5$ or $N_3O_2$ coordinating mode at the equatorial plane from ligand $L^1$ or $L^2$. Investigation over magnetic properties of these complexes reveals that the very weak magnetic coupling between neighboring Mn(II) ions connected by the diamagnetic dicyanidecobalt(III) building block. A best-fit to the magnetic susceptibility of complex ${\mathbf}{1}$ leads to the magnetic coupling constants $J=-0.084(3)cm^{-1}$.

Synthesis and Properties of Hyperbranched Polyester with Second-Order Outical Nonlinearity (2차 비선형 광학 초분지형 폴리에스테르의 합성 및 특성)

  • 이종협;이광섭
    • Polymer(Korea)
    • /
    • v.25 no.6
    • /
    • pp.803-810
    • /
    • 2001
  • A nonlinear optical hyperbranched polyester (PE-Azo/Hyper) was synthesized from 4-[N,N-bis(hydroxyethyl)amino-4'-formyl] azobenzene and cyanoacetic acid by a Knoevenagel polycondensation using 4-(dimethylamino) pyridine as a base. The resulting polymer was soluble in polar aprotic solvents such as N,N-dimethylformamide and 1-methyl-2-pyrrolidinone and could be processed into optical quality films by spin coating. The molecular weight was determined to be $M_w$=61,800 ($M_W/M_n{=1.86}$) by gel permeation chromatography using polystyrene as a standard. No melting point was detected by differential scanning Calorimeter, indicating that this polymer presents an amorphous state. It shows a glass transition temperature of $121^{\circ}C$. The second-order nonlinear optical coefficient $d_{33}$ of the poled polymer determined by the second harmonic generation at 1064 nm was 25.4 pm/V.

  • PDF

Reaction of Bis(diethylamino)aluminum Hydride in Tetrahydrofuran with Selected Organic Compounds Containing Representative Functional Groups

  • Jin Soon Cha;Oh Oun Kwon;Jong Mi Kim
    • Bulletin of the Korean Chemical Society
    • /
    • v.15 no.2
    • /
    • pp.132-138
    • /
    • 1994
  • Bis(diethylamino)aluminum hydride was utilized in a systematic study of the approximate rates and stoichiometry of the reaction of excess reagent with 55 selected organic compounds containing representative functional groups under standardized conditions (THF, $0^{\circ}C$, reagent to compound=4 : 1) in order to define the characteristics of the reagent for selective reductions. The reducing action of BEAH was also compared with that of the parent aluminum hydride. The reducing action of the reagent is quite similar to that of aluminum hydride, but the reducing power is much weaker. Aldehydes and ketones were readily reduced in 1-3 h to the corresponding alcohols. However, unexpectedly, a ready involvement of the double bond in cinnamaldehyde was realized to afford hydrocinnamyl alcohol. The introduction of diethylamino group to the parent aluminum hydride appears not to be appreciably influential in stereoselectivity on the reduction of cyclic ketones. Both p-benzoquinone and anthraquinone utilized 2 equiv of hydride readily without evolution of hydrogen, proceeded cleanly to the 1,4-reduction products. Carboxylic acids and acid chlorides underwent reduction to alcohols slowly, whereas cyclic anhydrides utilized only 2 equiv of hydride slowly to the corresponding hydroxylacids. Especially, benzoic acid with a limiting amount of hydride was reduced to benzaldehyde in a yield of 80%. Esters and lactones were also readily reduced to alcohols. Epoxides examined all reacted slowly to give the ring-opened products. Primary and tertiary amides utilized 1 equiv of hydride fast and further hydride utilization was quite slow. The examination for possibility of achieving a partial reduction to aldehydes was also performed. Among them, benzamide and N,N-dimethylbenzamide gave ca, 90% yields of benzaldehyde. Both the nitriles examined were also slowly reduced to the amines. Unexpectedly, both aliphatic and aromatic nitro compounds proved to be relatively reactive to the reagent. On the other hand, azo- and azoxybenzenes were quite inert to BEAH. Cyclohexanone oxime liberated 1 equiv of hydrogen and utilized 1 equiv of hydride for reduction, corresponding to N-hydroxycyclohexylamine. Pyridine ring compounds were also slowly attacked. Disulfides were readily reduced with hydrogen evolution to the thiols, and dimethyl sulfoxide and diphenyl sulfone were also rapidly reduced to the sulfides.

Carbonic Anhydrase Mimicry for Carbon Dioxide Fixation and Calcium Carbonate Mineralization (탄산탈수효소 모사를 이용한 이산화탄소 고정화 및 탄산칼슘 합성)

  • Sahoo, Prakash C.;Jang, Young Nam;Chae, Soo Chun;Lee, Seung Woo
    • Particle and aerosol research
    • /
    • v.9 no.4
    • /
    • pp.201-208
    • /
    • 2013
  • Copper (II) and Nickel (II) mimic complexes of enzyme carbonic anhydrase were evaluated under ambient condition for carbon dioxide capture and conversion process. The synthesized complexes were characterized by ATR-FTIR and UV-DR spectroscopy. It was found that all the complexes have biomimetic activity towards $CO_2$ using para-nitrophenyl acetate (p-NPA) hydrolysis as the model reaction. Interestingly, the proper geometry obtained by the restricted orientation of tripodal N atoms in Cu (II) complex of 2,6-bis(2-benzimidazolyl) pyridine showed the highest activity (1.14 au) compared to others. The $CO_2$ bio-mineralization to $CaCO_3$ was carried out via in-vitro crystallization approach. Results indicate that the biomimetic complexes have a role in determining $CaCO_3$ morphology. The present observations establish a qualitative insight for the design of improved small-molecule catalysts for carbon capture.