• Bulletin of the Korean Chemical Society
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• v.30 no.8
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• pp.1711-1714
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• 2009

We have described an efficient synthesis of quino[2,3-b][1,5]benzoxazepine α-aminophosphonate derivatives by the nucleophilic addition of triethyl phosphite to substituted quino[2,3-b][1,5]benzoxazepines promoted by easily available, inexpensive and mild catalyst KAl(S$O_4)_2{\cdot}12H_2$O(alum). The reactions proceed smoothly at room temperature under solvent-free reaction conditions and providing high yield of product in very short reaction time.

• Bulletin of the Korean Chemical Society
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• v.30 no.5
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• pp.1054-1056
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• 2009

We have demonstrated a one-pot three component coupling of an aldehydes, an amines, and triethyl phosphite using 1-benzyl-3-methyl imidazolium hydrogen sulphate [bnmim][][$HSO_{4}$] as an efficient catalyst. All the reactions proceed under solvent-free conditions at room temperature. This methodology afforded the corresponding $\alpha$-aminophosphonates in shorter reaction times with excellent yields.

• Bulletin of the Korean Chemical Society
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• v.29 no.9
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• pp.1752-1754
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• 2008

A simple and efficient synthesis of 3,4-dihydropyrimidinones or thiones is described, using silica-supported perchloric acid ($HClO_4-SiO_2$) as a heterogeneous catalyst from an aldehyde, $\beta$-dicarbonyl compound, and urea or thiourea under solvent-free conditions. Compared to the classical Biginelli reactions, this method consistently has the advantage of high yields, short reaction time, easy separation, and tolerance towards various functional groups.

• Bulletin of the Korean Chemical Society
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• v.27 no.1
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• pp.71-76
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• 2006

Porous polymer monolithic columns were prepared by the direct free radical copolymerization of methacrylic acid and ethylene glycol dimethacrylate within the confines of a chromatographic column in the presence of toluene-dodecanol as a porogenic solvent. The separation characteristics of the monolithic columns were tested by a homologous series of xanthine derivatives, theophylline and caffeine. The effects of the polymerization mixture composition and polymerization condition, mobile phase composition, flow rate and temperature on the retention times and separation efficiencies were investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and temperatures. Hydrogen-bonding interaction played an important role in the retention and separation. Compared with conventional particle columns, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency and fast analysis.

• Journal of the Korean Applied Science and Technology
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• v.18 no.2
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• pp.127-135
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• 2001

Alkyl polyglucosides were synthesized by solvent-free glycosidation using ultrasonic emulsification. We examined glycosidation conditions of fatty alcohol with glucose hydrate and anhydrous glucose in the presence of p-toluenesulfonic acid. Glucose was emulsified in a molar excess of fatty alcohol for 20 minutes with a ultra-sonicator at room temperature and converted in a stirred reactor to more than 95% polyglucoside within $2.5{\sim}3.5$ hr under $20{\sim}30$ mmHg at $110^{\circ}C$ with a three-fold molar ratio of fatty alcohol to glucose in the presence of 1mol% p-toluenesulfonic acid. It was possible to obtain a polyglucoside mixture of HLB 13 consisting of 65% monoglucoside and 35% oligoglucoside with less than 1% of fatty alcohol.

• Journal of Industrial and Engineering Chemistry
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• v.68
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• pp.153-160
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• 2018

An environmentally favorable (chlorine-free) solid oxidizer, guanidinium dinitramide [GDN; $NH_2C(NH_2)NH_2N(NO_2)_2$], was newly synthesized from guanidine carbonate [$NH_2C(=NH)NH_2{\cdot}1/2H_2CO_3$]. Two different crystalline forms (${\alpha}-type$ and ${\beta}-type$) appeared according to the applied solvents and synthesis conditions. Moisture, during extraction, might become trapped in a crystal between inner molecules. Therefore, despite having the same chemical composition, Raman-IR and TGA-DSC revealed different physical characteristics of the two forms. Peaks of Raman shift near $1000cm^{-1}$ implied different chemical structures. Thermal analysis revealed an exothermic temperature $155.7^{\circ}C$ for ${\alpha}-type$ but one of $191.6^{\circ}C$ for ${\beta}-type$. The caloric value of ${\alpha}-type$ was 536.4 J/g, which was 2.5 times larger than that of the ${\beta}-type$, which was 1310 J/g. While the synthesized GDN of ${\alpha}-type$ showed a steep exothermic decomposition, the ${\beta}-type$ was slowly decomposed after melting through an endothermic process. This work implied that despite of the same molecular formula some different core thermal properties would appear depending on synthesis conditions.

• Journal of Applied Biological Chemistry
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• v.63 no.1
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• pp.111-116
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• 2020

Total polyphenol contents, flavonoid contents, 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activities of ethanol extracts of 20 herbal plants (sage, turmeric, mace, bayleaf, fenugreek, oregano, blackpepper, whitepepper, clove, marjoram, cinnamon, coriander, basil, dillseed, mustard, cadamon, thyme, celery, rosemary, cumin) were analyzed for the screening of high flavonoid-containing plant resource. Thyme extract, showing the highest flavonoid content and a high degree of antioxidant activity, was selected as a bioactive cosmetic material. The total polyphenols and flavonoids contents of thyme extracts were measured as 6.90 mg chlorogenic acid equivalent (CAE)/100 g and 1.71 mg naringin equivalent (NE)/100 g, respectively, and DPPH radical scavenging activities was 90%. Among the tested organic solvents, hexane gave the highest extraction yield. Thus hexane was selected as the most suitable solvent for the extraction of thyme. Response surface method was used to obtain optimized extraction conditions for thyme: reaction temperature of 35.9 ℃, raw material to hexane ratio of 1.63:25 (w/v), and reaction time of 192 min. These predicted extraction conditions was validated by a total flavonoid extraction experiment showing a value equivalent to 96.3% of the predicted total flavonoid content. It is expected that the optimized solvent extraction conditions could be used for the production of flavonoid using thyme.

• Korean Journal of Food Science and Technology
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• v.38 no.4
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• pp.584-588
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• 2006

This study was carried out to optimize the conditions for the extraction of antioxidative materials from licorice root, Glycyrrhiz glabra. Chipped licorice roots were extracted with several solvents and their antioxidative activities were tested to determine the optimal extraction solvent. Among the solvents tested, 95% ethanol gave the highest free radical scavenging activity, and was therefore chosen as the optimal extracting solvent. The optimum extraction temperature and time were $20^{\circ}C$ and 12 hr, respectively. Next, the free radical scavenging activity of the ethanol extract was compared with that of other known antioxidants such as ${\alpha}-tocopherol$, butylated hydroxytoluene (BHT) and butylated hydroxyanisole (BHA). Ethanol extract of licorice root had greater antioxidative activity than ${\alpha}-tocopherol$ and a similar level to that of the two synthetic antioxidants (BHA and BHT). Moreover, the antioxidative activity of the ethanol extract was inhibited neither by heat treatment at $180^{\circ}C$ for 30 min nor by treatment at extreme pH. These findings suggest that ethanol extract of G. glabra may be useful as a natural antioxidant.

• Polymer(Korea)
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• v.28 no.2
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• pp.103-110
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• 2004

The biodegradable poly($\varepsilon$-caprolactone) (PCL) microcapsules containing tocopherol were prepared by oil-in-water emulsion solvent evaporation method. The features of the microcapsules were investigated in the manufacturing conditions and degradation behaviors. The form and structural feature of the microcapsules were measured by scanning electron microscope and X-ray diffraction, respectively. The surface free energy of the microcapsules was executed using contact angle measurement. As a result, the microcapsules were more stable and spherical with poly(vinyl alcohol) given in a surfactant. The surface free energy and crystallinity of microcapsules were decreased with increasing the core concentration, and degradation of PCL was occurred after 21 days. The release behaviors were examined by Uv/vis. spectrophotometer. It was found that the release rate of the microcapsules was increased with increasing the stirring rate, due to the increased interface between microcapsules and release media.

• Journal of Microbiology and Biotechnology
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• v.31 no.3
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• pp.419-428
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• 2021

To efficiently recycle GH78 thermostable rhamnosidase (TpeRha) and easily separate it from the reaction mixture and furtherly improve the enzyme properties, the magnetic particle Fe3O4-SiO2-NH2-Cellu-ZIF8 (FSNcZ8) was prepared by modifying Fe3O4-NH2 with tetraethyl silicate (TEOS), microcrystalline cellulose and zinc nitrate hexahydrate. FSNcZ8 displayed better magnetic stability and higher-temperature stability than unmodified Fe3O4-NH2 (FN), and it was used to adsorb and immobilize TpeRha from Thermotoga petrophilea 13995. As for properties, FSNcZ8-TpeRha showed optimal reaction temperature and pH of 90℃ and 5.0, while its highest activity approached 714 U/g. In addition, FSNcZ8-TpeRha had better higher-temperature stability than FN. After incubation at 80℃ for 3 h, the residual enzyme activities of FSNcZ8-TpeRha, FN-TpeRha and free enzyme were 93.5%, 63.32%, and 62.77%, respectively. The organic solvent tolerance and the monosaccharides tolerance of FSNcZ8-TpeRha, compared with free TpeRha, were greatly improved. Using naringin (1 mmol/l) as the substrate, the optimal conversion conditions were as follows: FSNcZ8-TpeRha concentration was 6 U/ml; induction temperature was 80℃; the pH was 5.5; induction time was 30 min, and the yield of products was the same as free enzyme. After repeating the reaction 10 times, the conversion of naringin remained above 80%, showing great improvement of the catalytic efficiency and repeated utilization of the immobilized α-L-rhamnosidase.