• Bulletin of the Korean Chemical Society
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• v.20 no.10
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• pp.1153-1158
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• 1999

β-Cyclodextrin, amylose, and cellulose were partially methylated and acetylated in order to examine the relative reactivities of 2-, 3-, and 6-OH groups to alkylation and acylation. The partially methylated samples of the polysaccharides were treated with excess of ethyl iodide and sodium hydroxide in dimethyl sulfoxide to convert all of the free hydroxyl groups to ethyl ether groups. The partially O-ethylated and O-methylated polysaccharides were reductively cleaved with triethylsilane in the presence of trimethylsilyl methanesulfonate and borontrifluoride etherate (5 : 1 by mole) and the resulting 4-OH group was acetylated and benzoylated to form mixtures of eight 4-O-acyl-1,5-anhydroalditols. The relative ratio of the alditol esters were analyzed by gas chromatography to determine the degree of substitution at each position. A similar sequence of reactions was carried out with partially acetylated polysaccharides. The results indicated that the order of relative reactivities for methylation are 2-OH > 6-OH > 3-OH and for acylation are 6-OH > 2-OH > 3-OH regardless of the anomeric configuration.

• Bulletin of the Korean Chemical Society
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• v.19 no.12
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• pp.1355-1359
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• 1998

The treatment of 1,1-bis(phenylthio)-2,2,3,3,3-pentafluoropropylbenzene (1) with 2 equiv. of phenyllithium in THF at -78 ℃ resulted in the formation of isomeric mixture (70: 30) of trifluoromethylated 1,2-diphenylvinyl sulfide 2 in 87% yield. The further oxidation of 2 with m-chloroperbenzoic acid in methylene chloride afforded isomeric mixture (70:30) of trifluoromethylated 1,2-diphenylvinyl sulfone 3 in 87% yield. When 3 was reacted with carbon nucleophiles such as methyllithium, n-butyllithium, phenyllithium and lithium octylide, the corresponding addition-elimination adducts 4, 5, 6 and 7 were obtained in moderate to good yields. The reaction of 3 with 4 equiv. of tributyltin hydride in benzene at reflux temperature provided isomeric mixture (90 : 10) of trifluoromethylated 1,2-diphenylvinyl stannane 8 in 41% yield. The reaction of 8 with methyllithium in the presence of trimethylsilyl chloride gave isomeric mixtures (90: 10) of trifluoromethylated 1,2-diphenylvinyl silane 9 in 88% yield. Finally, the treatment of 8 with Br2 and 12 resulted in the formation of isomeric mixtures (90: 10) of trifluoromethylated 1,2-diphenylvinyl bromide 10 and iodide 11 in 72% and 90% yields, respectively.

• Bulletin of the Korean Chemical Society
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• v.22 no.12
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• pp.1385-1389
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• 2001

In situ generated homoallenylindium reagents derived from the reaction of indium with 4-bromo-3-[(tri-methylsilyl) methyl]-1,2-butadiene reacted with a variety of aldehydes in DMF to produce 2-(2-hydroxy-ethyl) homoallenylsilanes at room temperatu re in good to excellent yields. 2- or 3-Hydroxybenzaldehyde that contains labile hydrogen was reacted with homoallenylindium reagent to provide the homoallenylsilanes. In the case of 4-formylbenzoic acid, the desired compound was produced in 88% yield. 4-Bromo-3-[(trimethyl-silyl) methyl]-1,2-butadiene was prepared from monoacetylation and mesylation of 2-butyn-1,4-diol, addition of trimethylsilylmethyl anion, saponification and mesylation followed by Finkelstein reaction.

• Archives of Pharmacal Research
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• v.5 no.2
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• pp.71-77
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• 1982

Improvements in the analytical methodology used in the gas chromatographic/mass spectral analysis of phenolic compounds from cigarette smoke are described. For the direct analysis of crude samples, pyridine extraction and the glass capillary column GC was used for the separation of phenolics as trimethylsilyl derivativatives. The separations of cigarette smoke on Carbowax 20M and SE-54 wall coated open tubular columns are given. Improved methodology for the routine quantitation of the identified components using the computer-controlled multiple ion selection technique of MS presented. Considerations pertaining to routine analyses of a multitude of complex smoke samples are also discussed.

• Bulletin of the Korean Chemical Society
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• v.8 no.4
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• pp.270-272
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• 1987

1,1-Dichloro-2,3,4,5-tetraphenyl-1-silacyclopenta- 2,4-diene was synthesized through the reaction of $SiCl_4$ with 1,4-dilithiotetraphenylbutadiene in 50% yield. From the reaction of this silole with metal, an air sensitive red-brownish solid was obtained. Treatment of this reaction product with $CH_3I\; and\; Me_3SiCl$ gave 1,1-dimethyl-2,3,4,5-tetraphenyl-1-silacyclopenta- 2,4-diene and 1,1-bis(trimethylsilyl)-2,3,4,5-tetraphenyl-1-silacyclopenta-2,4-diene, respectively. From these results, the formation of reactive 2,3,4,5-tetraphenyl-1-silacyclopenta-2,4-dienyl dianion was confirmed.

• Bulletin of the Korean Chemical Society
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• v.8 no.5
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• pp.355-358
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• 1987

The reaction of t-butylithium with chlorodiphenylvinylsilane at low temperatures in hexane gave a 52% yield of the two isomeric 1,1,3,4-tetraphenyl-2,4-dineopenty-1,3-disilacyclo butanes mixture, formed by a head-to-tail dimerization of 1,1-diphenyl-2-neopentylsilene intermediate. In the presence of the trapping agents such as trimethylmethoxysilane and anthracene, the expected trapped adducts, 1-methoxy-l,l-diphenyl-2-trimethylsilyl-4,4-dimethyl-1-silapentane and 2,2-diphenyl-3-neopentyl-(5,6 : 7,8)-dibenzo-2-silabicyclo-(2.2.2)-octane, were obtained in 74% and 46% yields, respectively. These products were separated and their stereochemistry were assigned on the basis of $^1H$- and $^{13}C$-NMR data.

• Analytical Science and Technology
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• v.19 no.1
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• pp.103-106
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• 2006

A 35-year-old Perubian who suffered from grand mal seizures died in the aircraft on his way from the United States to Hongkong via Incheon international airport of Korea. While performing the autopsy, 115 packs made with double layer of transparent film and black plastic bag containing cocaine were found in the ileum and large intestine. Among of them, 3 packs were ruptured. To determine the concentration of cocaine and its metabolites, blood, urine, bile, liver, spleen, heart, kidney, brain and gastric contents were taken and toxicological analysis was performed. Gas chromatography/mass spectrometry (GC/MS) following liquid-phase extraction using chloroform:isopropanol (=9:1) and derivatization with bis(trimethylsilyl)-trifluoroacetamide (contains 1% trimethylchlorosilane) was performed. High levels of cocaine, benzoylecgonine (BE) and ecgonine methylester (EME) were found in the postmortem blood (0.96, 3.09 and $5.59{\mu}g/mL$) and urine (32.85, 145.35 and $53.17{\mu}g/mL$), respectively. Cocaine and its metabolites were also detected in all other biological specimen.

• Applied Chemistry for Engineering
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• v.26 no.4
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• pp.413-420
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• 2015

PTMSP-ZIF composite membranes were prepared by the addition of zeolitic imidazolate framework (ZIF-8) into poly (1-trimethylsilyl-1-propyne) (PTMSP) having high gas permeability to improve trade-off relationship of the polymer membrane. PTMSP-ZIF composite membranes were prepared with different amounts of ZIF-8; 0, 5, 10, 20, 30 and 40 wt%. Gas permeation properties for $H_2$, $N_2$, $CO_2$, and $CH_4$ were investigated by increasing the amount of ZIF-8 in the PTMSP. The gas permeability of PTMSP-ZIF composite membranes within 5~30 wt% of ZIF-8 contents increased as ZIF-8 contents went up and decreased thereafter. The gas permeability for $CO_2$ showed the maximum value of 76080 barrer at 30 wt% of ZIF-8 content and PTMSP-ZIF composite membrane containing 20 wt% of ZIF-8 content had the highest selectivity ($CO_2/N_2$) with the value of 8.2. The selectivity ($H_2/N_2$) and selectivity ($CO_2/CH_4$) were almost the same as PTMSP in the range 10~40 wt% of the ZIF-8. Overall, PTMSP-ZIF composite membranes resulted in maintained selectivity and increased permeability compared to those of PTMSP membranes.

• Journal of the Korean Electrochemical Society
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• v.20 no.2
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• pp.34-40
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• 2017

Electric double layer capacitors (EDLC: electric double layer capacitors) have drew attention as an energy storage device for the next generation because of their outstanding power capability and durability. But their usage is somewhat limited due to low energy density over secondary batteries. One of methods to improve the energy of EDLC is expanding the voltage window of cell operation by increasing the charge cut-off voltage. In this study, $SBP-BF_4$ (spirobipyrrolidinium tetrafluoroborate), $TEA-BF_4$ (tetraethylammonium tetraflouroborate) and $EMI-BF_4$ (1-ethyl-3-methylimidazolium tetrafluoroborate) in AN (acetonitrile) were selected to evaluate the possibility of application at high voltage environment. The LSV (linear sweep voltammetry) measurements showed that the 1.5M SBP-BF4/AN electrolyte was stable over a wide potential window and showed the best electrochemical performance compared to other combinations of electrolytes at high voltage environments (over 3.0 V). Furthermore, TMSP (tris(trimethylsilyl) phosphite) was applied to 1.5M SBP-BF4/AN in order to maintain stable performance at high voltage for the long period of time. The electrolyte with TMSP additive showed the capacity retention of 93% after 10,000 cycles at 3.3 V.

• Journal of the Korean Society of Clothing and Textiles
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• v.33 no.12
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• pp.2002-2010
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• 2009

The degradation behavior of berberine is examined using GC-MS to select the fingerprint products that can be used to identify berberine dye in badly faded archaeological textiles. A total of $100^{\circ}C$ thermal and $H_2O_2/UV/O_2$ degradation systems were used to degrade berberine chloride 0.1% solution up to 408 hours. The samples were analyzed using the GC-MS. Dihydroberberine, 2-pteridinamine, 6,7-dimethyl-N-[(trimethylsilyl) oxy]-, and 8-methoxy-11-[3-methylbutyl]-11H-indolo[3,2-c]-quinoline, 5-oxide were detected as the major products of thermal degradation and identified as the fingerprint products for berberine dye at the early stage of degradation. Isobenzofuran-1,3-dione,4,5-dimethoxy-, 9H-fluorene,3,6-bis(2-hydroxyethyl)-,1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro-, and 3-tert-butyl-4-hydroxyanisole were detected as the major products generated by the $H_2O_2/UV/O_2$ degradation and identified as the fingerprint products for berberine dye under severe degradation conditions.