• Title/Summary/Keyword: elemental analysis

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Carbonylative Cyclization of Unsaturated Carboxylic Acids by Palladium Complexes with Phosphines(I) Synthesis and Structure of Palladium(O, II) Complexes with Unsaturated Carboxylic Acids (포스핀류가 배위된 팔라듐 착물에 의한 불포화카르복실산의 카르보닐화고리 반응 (제 1 보). 불포화카르복실산이 배위된 팔라듐(0, Ⅱ) 착물의 합성과 구조)

  • Myung-Ki Doh;Maeng-Jun Jung;Dong-Jin Lee;Kohtaro Osakada;Akio Yamamoto
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.423-430
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    • 1993
  • New Palladium(0)-olefin complexes, $(PMe_3)_2Pd{CH_2=C(CH_3)COOH} \;and\;(PMe_3)_2Pd{(CH_3)CH=CHCOOH}$ have been prepared by treating $Pd(PMe_3)_2$(styrene) with methacrylic acid and trans-crotonic acid, respectively. These complexes were characterized by elemental analysis, IR and $^1H-,\;^{13}C-,\;and\;^{31}P$-NMR spectroscopy. The carboxylic acid entity was found non-bonded with palladium while ${\pi}$-bond is formed between the olefin double bond and Pd(0). The results are compared with the metallacycle formation the reaction of Pd(PMe3)2(styrene) with 3-butenoic acid.

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Synthesis, Characterization and Biological Studies of New Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide (2-(Benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene)acetohydrazide의 Mn(II), Ni(II), Co(II), Cu(II) 및 Zn(II) 착물의 합성, 특성 및 생물학적 연구)

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.;Al-Hakimi, Ahmed N.
    • Journal of the Korean Chemical Society
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    • v.55 no.1
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    • pp.19-27
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    • 2011
  • New series of Mn(II), Ni(II), Co(II), Cu(II) and Zn(II) of the 2-(benzothiazol-2-yl)-N'-(2,5-dihydroxybenzylidene) acetohydrazide have been synthesized and characterized by elemental analysis, IR, UV-vis, $^1H$-NMR, mass and ESR spectra, magnetic susceptibility and molar conductivity measurements. The spectral data and magnetic measurements of the complexes indicate that, the geometries are either square planar or octahedral. The biological activity of the ligand and its complexes against fungi (Aspergillus nigar and Fusarium oxysporium) were investigated. The metal complexes exhibited higher activity than both the parent ligand and the corresponding metal ion.

Some Pyridyl- and Thiophenyl-Substituted 1,2,4-Triazolo[3,4-b]1,3,4-thiadiazole Derivatives as Potent Antibacterial

  • Maqsood, Muhammad Rizwan;Hanif, Muhammad;Rafiq, Muhammad;Saleem, Muhammad;Zaib, Sumera;Khan, Aftab Ahmed;Iqbal, Mazhar;Iqbal, Jamshed;Rama, Nasim Hasan;Seo, Sung-Yum;Lee, Ki-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.4180-4184
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    • 2012
  • The target compounds 6-11a-e were synthesized by condensing 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones 5a-f with various aromatic carboxylic acids in the presence of phosphorous oxychloride. The structures of newly synthesized compounds were characterized by IR, $^1H$ NMR, $^{13}C$ NMR, elemental analysis and mass spectrometric studies. All the synthesized compounds were screened for their antibacterial activity. Almost all the tested compounds were potent against four different strains of bacteria when compared with that of reference drug ciprofloxacin. Compounds 6c, 6e, 8d, 9b, 9e, 11a and 11b showed nearly equal or lower MIC values than standard drug, against all four tested bacterial strains but rest of the compounds showed excellent antibacterial activities.

Synthesis and Biological Activities of Some New 3,6-Disubstituted 1,2,4-Triazolo[3,4-b]1,3,4-thiadiazole Derivatives

  • Rafiq, Muhammad;Saleem, Muhammad;Hanif, Muhammad;Maqsood, Muhammad Rizwan;Rama, Nasim Hasan;Lee, Ki-Hwan;Seo, Sung-Yum
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3943-3949
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    • 2012
  • A series of aromatic hydrazides 3a-j were prepared by refluxing esters 2a-j with hydrazine hydrate in methanol, which were prepared by the esterification of 1a-j. Acetohydrazides 3a-j upon treatment with carbon disulfide and methanolic potassium hydroxide yielded potassium dithiocarbazate salts 4a-j, which on refluxing with hydrazine hydrate yielded substituted 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones 5a-j. The target compounds 6a-j were synthesized by condensing furan-3-carboxylic acid in the presence of polyphosphoric acid under reflux. The structures of newly synthesized compounds were characterized by IR, $^1H$ NMR, $^{13}C$ NMR, elemental analysis and mass spectrometric studies. All the synthesized compounds were screened for their urease, acetylcholine esterase inhibition, antioxidant and alkaline phosphatase inhibition activity. Almost all of the compounds 6a-j showed good to excellent activities against urease and acetylcholine esterase more than the reference drugs. Compounds 6f and 6g were more potent scavenger of free radicals than the reference n-propyl gallate. Compound 6b and 6h showed excellent activities of alkaline phosphatase as compare to the reference $KH_2PO_4$.

Silica Sulfuric Acid as a Mild and Efficient Reagent for the Synthesis of 1,4-Diazepine and 1,5-Benzodiazepine Derivatives (Silica Sulfuric Acid를 이용한 효율적인 1,4-diazepine and 1,5-benzodiazepine 유도체의 합성)

  • Joshi, Y.C.;Saingar, Shalini;Kavita, Kavita;Joshi, P.;Kumar, Rajesh
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.638-643
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    • 2011
  • The synthesis of biologically active 1H-1,4-diazepines 4a-d and 3H-1,5-benzodiazepines 5a-d in good yields, from the heterocyclization reaction of 2-(4-methylthio benzenesulfonyl)-1,3-dimethyl/1-methyl-3-phenyl/1,3-diphenyl/1-methyl-3-ethoxy propane-1,3-dione 3a-d with ethylenediamine (EDA) and o-phenylenediamine (o-PDA), respectively, in the presence of silica sulfuric acid (SSA) is described. The novel ${\beta}$-diketones/${\beta}$-ketoesters 3a-d were synthesized by the condensation reaction of 4-methylthiobenzenesulfonyl chloride 1 with various ${\beta}$-diketones/${\beta}$-ketoesters 2a-d. All structures of the newly synthesized compounds were elucidated by elemental analysis and spectral studies. The compounds 4a-d and 5a-d have been screened for antimicrobial, antifungal and anthelmintic activity.

Synthesis and Characterization of a Novel Organotin Complex: Di(n-butyl) chloro[5-(p-dimethylaminobenzylidene)rhodanine]tin(IV) Based on a Competing N, O, and S Donor Ligand (새로운 유기주석 착물의 합성과 특성: 경쟁적인 N, O 및 S 주개 리간드에 기초한 Di(n-butyl)chloro[5-( p-dimethylaminobenzylidene)rhodanine]tin(IV))

  • Tarassoli, Abbas;Sedaghat, Tahereh;Mousavi, Fatemeh
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.590-593
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    • 2011
  • A novel organotin(IV) complex has been prepared from $Bu_2SnCl_2$ and the N, O and S donor ligand, 5-(p-dimethylaminobenzylidene) rodanine (HL). The ligand is deprotonated in the presence of a base and the complex with the general formula $SnBuCl_2L$ is formed. This complex was fully characterized by IR, $^1H$ NMR and $^{119}Sn$ NMR and elemental analysis. Spectroscopic data indicate the ligand is coordinated through the oxygen atom to the tin and the coordination number of four is supported by $^{119}Sn$ NMR data in solution.

Preparation and Unequivocal Identification of Chromophores-Substituted Carbosilane Dendrimers up to 7th Generations

  • Kim, Chung-Kyun;Kim, Hyo-Jung;Oh, Myeong-Jin;Hong, Jang-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.30 no.4
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    • pp.873-881
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    • 2009
  • Bis(phenylethynyl)dimethylsilane is branched by the hydrosilation of the phenylethynyl group with dichloromethylsilane, and then the resulting chlorosilane is reacted with lithium phenylacetylide to give the $1^{st}$ generation. The same hydrosilation and alkynylation are repeated to obtain the $7^{th}$ generation. In addition peripheral Si-Cl moiety of the seven kind generation dendrimers are reacted with alcoholic moiety of 9-hydroxymethylanthracene and 2-(2-hydroxyphenyl)benzoxazole group in the presence of TMEDA. Then three kinds of carbosilane dendrimers are prepared from the $1^{st}$ to the $7^{th}$ generations, the $7^{th}$ generation of each dendrimer has 256 phenylethynyl, 256 9-anthracenylmethoxy, or 128 2-(2-phenoxy)benzoxazole groups. Each synthesized dendrimer is unequivocally characterized by $^1H\;and\;^{13}C\;NMR$, elemental analysis, MALDI-MS, GPC, and PL (photoluminescence). Characteristically PDI (Polydisperse Index) values of the dendrimers’ peak in GPC are in the range of $1.00{\sim}1.07$, which indicates that each generation of carbosilane is in unified distribution. PL spectra of phenylethynyl and 9- anthracenemethoxy group substituted dendrimers show no significant change with increasing the generation from the $1^{st}$ to the $7^{th}$. However, the PL spectra of 2-(2-phenoxy)benzoxazole group substituted dendrimers show a blue-shift trend with increasing the generation from the $1^{st}$ to the $7^{th}$.

Titanized or Zirconized Porous Silica Modified with a Cellulose Derivative as New Chiral Stationary Phases

  • Seo, You-Jin;Kang, Gyoung-Won;Park, Seong-Tae;Moon, Myeong-Hee;Park, Jung-Hag;Cheong, Won-Jo
    • Bulletin of the Korean Chemical Society
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    • v.28 no.6
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    • pp.999-1004
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    • 2007
  • Spherical porous silica supports modified with titanium or zirconium alkoxides were prepared, and allyl groups were chemically attached to the titanized or zirconized silica supports, and the product was cross-polymerized with a double bond containing cellulose derivative to yield new CSPs (chiral stationary phases). Magic angle spinning 13C solid state NMR and elemental analysis were used to characterize the CSPs. The performances of the chiral stationary phases were examined in comparison with a conventional chiral stationary phase. Spherical porous silica particles modified with 3,5-dimethylphenylcarbamate of cellulose were prepared and used as the conventional chiral stationary phase. Chromatographic data were collected for a few pairs of enantionmers in heptane/2-propanol mixed solvents of various compositions with the three chiral columns and the results were comparatively studied. The separation performance of the chrial phase made of the titanized silica was better than the others, and the separation performance of the chiral phase of the zirconized silica was comparable to that of the conventional chiral phase. The superiority of titanized silica over bare or zirconized silica in chiral separation seemed to be owing to the better yield of crosslinking (monitored by increase of carbon load) for titanized silica than for the others.

Clean and Efficient Synthesis of Furfural From Xylose by Microwave-Assisted Biphasic System using Bio-Based Heterogeneous Acid Catalysts

  • Vo, Anh Thi Hoang;Lee, Hong-shik;Kim, Sangyong;Cho, Jin Ku
    • Clean Technology
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    • v.22 no.4
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    • pp.250-257
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    • 2016
  • As an attempt to replacing petroleum-based chemicals with bio-based ones, synthesis of furfural from biomass-derived xylose attracts much attention in recent days. Conventionally, furfural from xylose has been produced via the utilization of highly corrosive, toxic, and environmentally unfriendly mineral acids such as sulfuric acid or hydrochloric acid. In this study, microwave-assisted biphasic reaction process in the presence of novel bio-based heterogeneous acid catalysts was developed for the eco-benign and effective synthesis of furfural from xylose. The microwave was irradiated for reaction acceleration and a biphasic system consisting of $H_2O$ : MIBK (1 : 2) was designed for continuous extraction of furfural into the organic phase in order to reduce the undesired side products formed by decomposition/condensation/oligomerization in the acidic aqueous phase. Moreover, sulfonated amorphous carbonaceous materials were prepared from wood powder, the most abundant lignocellulosic biomass. The prepared catalysts were characterized by FT-IR, XPS, BET, elemental analysis and they were used as bio-based heterogeneous acid catalysts for the dehydration of xylose into furfural more effectively. For further optimization, the effect of temperature, reaction time, water/organic solvent ratio, and substrate/catalyst ratio on the xylose conversion and furfural yield were investigated and 100% conversion of xylose and 74% yield of furfural was achieved within 5 h at $180^{\circ}C$. The bio-based heterogeneous acid catalysts could be used three times without any significant loss of activity. This greener protocol provides highly selective conversion of xylose to furfural as well as facile isolation of product and bio-based heterogeneous acid catalysts can alternate the environmentally-burdened mineral acids.

Efficacy of various cleaning solutions on saliva-contaminated zirconia for improved resin bonding

  • Kim, Da-Hye;Son, Jun-Sik;Jeong, Seong-Hwa;Kim, Young-Kyung;Kim, Kyo-Han;Kwon, Tae-Yub
    • The Journal of Advanced Prosthodontics
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    • v.7 no.2
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    • pp.85-92
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    • 2015
  • PURPOSE. This study aimed to investigate the efficacy of cleaning solutions on saliva-contaminated zirconia in comparison to air-abrasion in terms of resin bonding. MATERIALS AND METHODS. For saliva-contaminated air-abraded zirconia, seven cleaning methods)-no contamination (NC), water-spray rinsing (WS), additional air-abrasion (AA), and cleaning with four solutions (Ivoclean [IC]; 1.0 wt% sodium dodecyl sulfate [SDS], 1.0 wt% hydrogen peroxide [HP], and 1.0 wt% sodium hypochlorite [SHC])-were tested. The zirconia surfaces for each group were characterized using various analytical techniques. Three bonded resin (Panavia F 2.0) cylinders (bonding area: $4.5mm^2$) were made on one zirconia disk specimen using the Ultradent jig method [four disks (12 cylinders)/group; a total of 28 disks]. After 5,000 thermocycling, all specimens were subjected to a shear bond strength test with a crosshead speed of 1.0 mm/minute. The fractured surfaces were observed using an optical and scanning electron microscope (SEM). RESULTS. Contact angle measurements showed that groups NC, AA, IC, and SHC had hydrophilic surfaces. The X-ray photoelectron spectroscopy (XPS) analysis showed similar elemental distributions between group AA and groups IC and SHC. Groups IC and SHC showed statistically similar bond strengths to groups NC and AA (P>.05), but not groups SDS and HP (P<.05). For groups WS, SDS, and HP, blister-like bubble formations were observed on the surfaces under SEM. CONCLUSION. Within the limitations of this in vitro study, some of the cleaning solutions (IC or SHC) were effective in removing saliva contamination and enhancing the resin bond strength.