• Journal of the Korean Chemical Society
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• v.56 no.4
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• pp.440-447
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• 2012

Heteroleptic complexes of zirconium (IV) derived from bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic ${\beta}$-diketones of the general formula ZrLL' (where $LH_2=RCNH(C_6H_4)SC:C(OH)N(C_6H_5)N:CCH_3$, $R=-C_6H_5$, $-C_6H_4Cl(p)$ and $L^{\prime}H_2=R^{\prime}C:(NOH)C:C(OH)N(C_6H_5)N:CCH_3$, $R^{\prime}=-CH_2CH_3$, $-C_6H_5$, $-C_6H_4Cl(p)$ were prepared by the reactions of zirconium tetrachloride with disodium salts of Schiff bases ($L\;Na_2$) and oximes of heterocyclic ${\beta}$-diketones ($L^{\prime}\;Na_2$) in 1:1:1 molar ratio in dry refluxing THF. The structures of these monomeric zirconium (IV) complexes were elucidated with the help of elemental analysis, molecular weight measurements, spectroscopic (IR, NMR and mass) studies. A distorted trigonal bipyramidal geometry may be suggested for these heteroleptic zirconium (IV) complexes. The ligands (bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic ${\beta}$-diketones) and their heteroleptic complexes of zirconium (IV) were screened against A. flavus, P. aeruginesa and E. coli.

• Bulletin of the Korean Chemical Society
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• v.35 no.10
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• pp.2917-2921
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• 2014

Cerium-activated yttrium aluminate ($Y_3Al_5O_{12}:Ce^{3+}$) exhibiting a garnet structure has been widely utilized in the production of light emitting diodes (LEDs) as a yellow emitting phosphor. The commercialized yttrium aluminum garnet (YAG) phosphor is typically synthesized by a solid-state reaction, which produces irregular shape particles with a size of several tens of micrometers by using the top-down method. To control the shape and size of particles, which had been the primary disadvantage of top-down synthetic methods, we synthesized YAG:Ce nanoparticles with a diameter of 500 nm using a coprecipitation method under the atmospheric pressure without the use of template or special equipment. The precursor particles were formed by refluxing an aqueous solution of the nitrate salts of Y, Al, and Ce, urea, and polyvinylpyrrolidone (55 K) at $100^{\circ}C$ for 12 h. YAG:Ce nanoparticles were formed by the calcination of precursor particles at $1100^{\circ}C$ for 10 h under atmospheric conditions. The phase identification, microstructure, and photoluminescent properties of the products were evaluated by X-ray powder diffraction, scanning electron microscopy, absorption spectrum and photoluminescence analyses.

• Journal of the Korean Chemical Society
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• v.57 no.5
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• pp.612-617
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• 2013

The versatile, hitherto unreported 3-(4-(2-phenyldiazenyl)-2-oxo-2H-chromen-3-yl)-3-oxopropanenitrile 3 was prepared by two convenient routes: either by the reaction of ethyl 4-(2-phenyldiazenyl)-2-oxo-2H-chromen-3-carboxylate 2 with acetonitrile in the presence of sodium hydride or by treatment of 4-(2-phenyldiazenyl)-3-(2-bromoacetyl)-2H-chromen-2- one 5 with potassium cyanide. Reaction of 3 with heterocyclic diazonium salts 6, 7, 14 and 17 furnished the corresponding hydrazones 8, 9, 15 and 18. The latter hydrazones underwent intramolecular cyclization into the corresponding pyrazolo[5,1- c]-1,2,4-triazine 10, 1,2,4-triazolo[5,1-c]-1,2,4-triazine 11, 1,2,4-triazino[4,3-b]indazole 16 and imidazo[2,1-c]-1,2,4-triazine 19 derivatives, respectively upon refluxing in pyridine.

• Journal of the Korean Chemical Society
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• v.5 no.1
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• pp.60-65
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• 1961

Nowadays, it is a well-known fact that the epoxy resins play an important role in the industrial field of plastics because of their excellent properties. Although studies on the polymers of epichlorohydrin with phenols, up-to-date, were various, there were only a few wokrs on the polymers of epichlorohydrin with amines. Therefore the experiments are carried out about the polymerization of epichlorohydrin with ${\alpha}-, {\beta}$-naphtylamine, o-, m-, p-toluidine, and o-, m-, p-nitroaniline. Examining the polymerization processes and the differences in the properties of the polymers, we obtained the following conclusions. 1) ${\alpha}$-naphthylamine, ${\beta}$-naphthylamine, o-toluidine, m-toluidine and p-toluidine react with epichlorohydrin to form polymers but o-, m-, and p-nitroaniline do not make polymers with epichlorohydrin. 2) As polymerization times after adding sodium hydroxide and refluxing again 3hrs. are suitable for ${\alpha}$-naphthylamine-epichlorohydrin, 3.5hrs. for${\beta}$-naphthylamine-epichlorohydrin, and 4hrs, for m-toluidine-epichlorohydrin. 3) Method for determining molecular weight of these polymers by the titration of end group is applicable to the polymers having D.P. less than about 200 for ${\alpha}$-, ${\beta}$-naphthylamine-epichlorohydrin and those having D.P. less than 18 for m-toluidine-epichlorohydrin. 4) Gererally, these polymers get special colors so that these need proper pigmentation to use as molding compounds.

• YAKHAK HOEJI
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• v.36 no.4
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• pp.350-356
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• 1992

Anticoagulant activities were tested for the fifteen kinds of medicinal plants by measuring activated partial thromboplastin time (aPTT). Of them five kinds or species (Artemisia princeps, Sanguisorba officinalis, Artemisia apiacea, Eclipa alba, Schizonepeta tenuifolia) were selected and fractionated for the preparation of acidic polysaccharides. They were extracted with water by refluxing and the extracts were precipitated with ethanol. The precipitates were separated based on charge using a DEAE-Sephadex. The low salt and high salt fractions were sulfated with anhydrous pyridine and chlorosulfonic acid complex. In vitro anticoagulant activities of sulfated polysaccharides were tested by measuring aPTT, prothrombin time (PT), and factor Xa clotting time using normal human plasma. No relationship was found between the amount of uronic acids and anticoagulant activities, but the sulfated ones show the increase of activities. In vivo anticoagulant properties of the sulfated polysaccharide from Artemisia apiacea were also tested by the intraveneous administration of three different doses (3,5 and 10 mg/kg) to rats. APTT and PT were increased significantly and the action of factor Xa and thrombin mediated through antithrombin III were inhibited slightly.

• Biomedical Science Letters
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• v.27 no.2
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• pp.77-87
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• 2021

Reflux esophagitis (RE) is a disease that stomach contents, stomach acid, and pepsin continually refluxing and is curently increasing worldwide. This study was conducted to find natural materials that can reduce side effects and effectively treat RE. Animal experiments were conducted with a 1:1 (EA1), 1:5 (EA5) ratio of Evodiae Fructus and Arecae Semen known to be effective against reflux esophagitis. As a result of confirming the total lesion of the esophageal mucosa after EA1 or EA5 treatment in reflux esophagitis animals, it showed superior improvement compared to the RE-control rats. In addition, by regulating the expression of MPO and NADPH oxidase, the activation of NF-κB was inhibited, and the expression of COX-1 and COX-2 was regulated. Moreover, its improved esophageal barrier function through regulating protein expressions of tight junction protein and MMPs/TIMPs. Taken together, a mixture of Evodiae Fructus and Arecae Semen can attenuate the damage to the esophageal mucosa that not only inactivationed the NF-κB through oxidative stress control, but also by regulating tight junctions and MMPs/TIMPs. This effect was more excellent in the 1:1 mixture (EA1) than in the Evodiae Fructus and Arecae Semen 1:5 mixture (EA5).

• Preventive Nutrition and Food Science
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• v.5 no.1
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• pp.10-14
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• 2000

A simple and rapid method was developed to prepare a large quantity of highly pure conjugated linoleic acid (CLA) chemically-synthesized from safflower seed oil (SSO). CLA-SSO(74.9% in purity) was synthesized from fresh SSO(79.9% of linoleic acid) by alkaline isomerization at 18$0^{\circ}C$. Urea(50g) and CLA-SSO (25g) were completely dissolved in ethanol (750ml) using a water bath(5$0^{\circ}C$) and followed by refluxing for 60 min. The resultant was cooled to room temperature and stored in a cold room (4$^{\circ}C$) for 24hrs. After removing the urea adduct by filtration, the filtrate was rotoevaporated under 4$0^{\circ}C$ and the residue was dissolved in hexane (200ml). The hexane extract was washed with distilled water (100ml$\times$3) and dried over sodium sulfate anhydrous. This urea treatment procedure was repeated three times. The purity of CLA recovered from the hexane extract was 95.0%. This method can be applied to prepare a large quantity of highly pure chemically-synthesized CLA (>0.5kg/a batch) from any plant oils containing high percentages (>70%) of linoleic acid.

• Archives of Pharmacal Research
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• v.13 no.4
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• pp.351-354
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• 1990

2, 3-diphenyl-4-cyano-pyrrole-5-thione (4) was either by the reaction of benzoin (1) and cyanothioacetamide (3) followed by cyclization using AcOH/sodium acetate or by refluxing a mixture of benzoin (1) and cyanothioacethamide in pyridine to afford directly 4. Several new pyrrole and pyrazole derivatives were synthesised using 4 as synthon. The structure of the newly synthesised derivatives were based on celemental and spectral data studies. Methylation of the SH group in 4 afforded 5. Reaction of 4 with ethyl bromo acetate afforded (6). Treatment of (5) and (6) with hydrazine hydrate afforded the same pyrazole derivative (10) through the intermediate (9). Treatment of 6 with aniline and phenylhydrazine afforded the pyrrole derivatives 8a, b respectively. Treatment of 6 while dill HCI gave 2, 3-diphenyl-4-cyano-pyrrole-5-one (7). Treatment of 6 with $NH_3$/EtOH afforded the amidic derivatives (11) with treatment of 6 $NH_3$/ heat then acidification it gave the carboxylic derivatives (12).

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.483-487
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• 1986

The synthesis of $\beta-damascone$ (I), an odoriferous natural product, was investigated from 2,2,6-trimethylcyclohexanone (II); (II) was ethynylated by the action of monoacetylide anion prepared from acetylene and sec-butyllithium at -78${\circ}C$, to give an ethynylcarbinol(III), which was isomerized to an acetylcyclohexene(IV) by refluxing in aqueous oxalic or formic acid. (IV) was treated with sec-butyllithium, the enolate was reacted with freshly dried acetaldehyde, and the resultant $\beta-hydroxyketone$ (V) was dehydrated by TsOH to ${\beta}$-damascone, trans-2,6,6-trimethyl-1-crotonyl-1-cyclohexene(I).

• Journal of the Korean Chemical Society
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• v.38 no.12
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• pp.880-884
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• 1994

An indirect spectrophotometric method, presumably heretofore unmentioned, for the rapid determination of COD in the presence of chloride of high concentration is described. The alkaline sample is refluxed to react with a definite amount of permanganate, present in excess. A photometric measurement at 535 nm for the extent of the fading of the permanganate color after refluxing completes the procedure. The optimum conditions which give the absorbance-concentration plot the maximum linearity and slope in the range of 0∼5 ppm COD are as follows: reflux at $100\circC$ for 10 min in the presence of 0.15 mM permanganate and 0.2% NaOH with a sample size of 5 ml. An overall running time was less than 15 min. The t-test reveals that the proposed method is not significantly different from the official method.