• Title/Summary/Keyword: 2-$c$]pyridine

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Optimization of Conditions for the Microencapsulation of ${\alpha}-Tocopherol$ and Its Storage Stability (${\alpha}-Tocopherol$ 미세캡슐화의 최적화 및 저장안정성 규명)

  • Chang, Pahn-Shick;Ha, Jae-Seok;Roh, Hoe-Jin;Choi, Jin-Hwan
    • Korean Journal of Food Science and Technology
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    • v.32 no.4
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    • pp.843-850
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    • 2000
  • We have produced the microcapsule composed of ${\alpha}-tocopherol$ as a core material (Cm) and the gelatinized polysaccharide as a wall material (Wm). Firstly, we have developed a simple, sensitive, and quantitative analysis method of the microencapsulation product using 5% cupric acetate pyridine solution. We could then optimize all the conditions for the microencapsulation process such as the ratio of [Cm] to [Wm], the temperature of dispersion fluid, and the emulsifier concentration using response surface methodology (RSM). As for the microencapsulation of ${\alpha}-tocopherol$, the regression model equation for the yield of microencapsulation (YM, %) to the change of an independent variable could be predicted as follows : YM=99.77-1.76([Cm]:[Wm])-1.72$([Cm]\;:\;[Wm])^2$. From the ridge of maximum response, the optimum conditions for the microencapsulation of ${\alpha}-tocopherol$ were able to be determined as the ratio of [Cm] to [Wm] of 4.6:5.4(w/w), the emulsifier concentration of 0.49%, and dispersion fluid temperature of $25.5^{\circ}C$, respectively. Finally, the microcapsules produced under the optimal conditions were applied for the analysis of storage stability. The optimal conditions for the storage were found to be the values of pH 9.0 and $25{\sim}35^{\circ}C$. And the storage stability of the microcapsules containing ${\alpha}-tocopherol$ were higher than 99% for a week at pH 9.0 and $25^{\circ}C$.

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1,1-Difluoroethane Synthesis from Acetylene over Fluorinated γ-Al2O3 (불화된 γ-Al2O3상에서 아세틸렌으로부터 1,1-difluoroethane의 합성)

  • Lee, Youn-Woo;Lee, Kyong-Hwan;Lim, Jong Sung;Kim, Jae-Duck;Lee, Youn Yong
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.629-633
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    • 1998
  • The synthesis of 1,1-difluoroethane from acetylene as a function of HF/acetylene ratio, contact time and reaction temperature was studied on a fluorinated ${\gamma}-Al_2O_3$. The fluorination of ${\gamma}-Al_2O_3$ was treated with pure HF gas at high temperature. The crystallinity, the porosity, and the acid properties of the prepared samples were examined using XRD, the nitrogen adsorption, pyridine-IR and ammonia-TPD respectively. The activity was enhanced by further fluorination of alumina. The fraction of 1,1-difluoroethane was obtained above 90% at reaction temperature of about $200^{\circ}C$. The ratio of 1,1-difluoroethane to vinylfluoride over fluorinated ${\gamma}-Al_2O_3$ catalyst was increased with the mole ratio of HF/acetylene and contact time, and was found to be the highest ratio at reaction temperature of $200^{\circ}C$.

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Reaction of Potassium 2-Thexyl-1,3,2-dioxaborinane Hydride with Selected Organic Compounds Containing Representative Functional Groups

  • Jin Soon Cha;Sung Eun Lee
    • Bulletin of the Korean Chemical Society
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    • v.13 no.5
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    • pp.531-537
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    • 1992
  • The approximate rates and stoichiometry of the reaction of excess potassium 2-thexyl-1,3,2-dioxaborinane hydride(KTDBNH) with 55 selected compounds containing representative functional groups under standardized conditions (tetrahydrofuran, TEX>$0^{\circ}C$, reagent : compound=4 : 1) was examined in order to define the characteristics of the reagent for selective reductions. Benzyl alcohol and phenol evolve hydrogen immediately. However, primary, secondary and tertiary alcohols evolve hydrogen slowly, and the rate of hydrogen evolution is in order of $1^{\circ}$> $2^{\circ}$> $3^{\circ}$. n-Hexylamine is inert toward the reagent, whereas the thiols examined evolve hydrogen rapidly. Aldehydes and ketones are reduced rapidly and quantitatively to give the corresponding alcohols. Cinnamaldehyde is rapidly reduced to cinnamyl alcohol, and further reduction is slow under these conditions. The reaction with p-benzoquinone dose not show a clean reduction, but anthraquinone is cleanly reduced to 9,10-dihydro-9,10-anthracenediol. Carboxylic acids liberate hydrogen immediately, further reduction is very slow. Cyclic anhydrides slowly consume 2 equiv of hydride, corresponding to reduction to the caboxylic acid and alcohol stages. Acid chlorides, esters, and lactones are rapidly and quantitatively reduced to the corresponding carbinols. Epoxides consume 1 equiv hydride slowly. Primary amides evolve 1 equiv of hydrogen readily, but further reduction is slow. Tertiary amides are also reduced slowly. Both aliphatic and aromatic nitriles consume 1 equiv of hydride rapidly, but further hydride uptake is slow. Analysis of the reaction mixture with 2,4-dinitrophenylhydrazine yields 64% of caproaldehyde and 87% of benzaldehyde, respectively. 1-Nitropropane utilizes 2 equiv of hydride, one for hydrogen evolution and the other for reduction. Other nitrogen compounds examined are also reduced slowly. Cyclohexanone oxime undergoes slow reduction to N-cyclohexylhydroxyamine. Pyridine ring is slowly attacked. Disulfides examined are reduced readily to the correponding thiols with rapid evolution of 1 equiv hydrogen. Dimethyl sulfoxide is reduced slowly to dimethyl sulfide, whereas the reduction of diphenyl sulfone is very slow. Sulfonic acids only liberate hydrogen quantitatively without any reduction. Finally, cyclohexyl tosylate is inert to this reagent. Consequently, potassium 2-thexyl-1,3,2-dioxaborinane hydride, a monoalkyldialkoxyborohydride, shows a unique reducing characteristics. The reducing power of this reagent exists somewhere between trialkylborohydrides and trialkoxyborohydride. Therefore, the reagent should find a useful application in organic synthesis, especially in the field of selective reduction.

Optimization of Fish Oil Microencapsulation by Response Surface Methodology and Its Storage Stability (반응표면분석법에 의한 정제어유 미세캡슐화 공정의 최적화 및 미세캡슐 저장안정성 분석)

  • Chang, Pahn-Shick;Ha, Jae-Seok
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.646-653
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    • 2000
  • Using agar and waxy com starch as the wall material, we could encapsulate the purified fish oil. Firstly, we have developed a simple and sensitive method for the quantitative analysis of the microencapsulation yield using 5% cupric acetate pyridine solution. Then, the optimum conditions such as the ratio of [core material] to [wall material]$(X_1)$, the temperature of dispersion fluid$(X_2)$, and the emulsifier concentration$(X_3)$ for the microencapsulation process were determined by using response surface methodology(RSM). The regression model equation for the yield of microencapsulation(Y, %) of purified fish oil upon three kinds of independent variables could be predicted as follows; Y = 100.138621-0.735000$(X_1)$+0.840000$(X_1)(X_2)$+0.817500$(X_1)(X_3)$-0.852500$(X_2)(X_3)$. And the optimum conditions for the microencapsulation of the purified fish oil were the ratio of [core material] to [wall material] of 4.9 : 5.1(w/w), the emulsifier concentration of 0.48%, and dispersion fluid temperature of $19.4^{\circ}C$. The microcapsules containing the purified fish oil showed the highest storage stability at pH 7.0 and $20{\sim}25^{\circ}C$.

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Changes of Aroma and Volatile Components of Korean Leaf Tobaccos from a Different Stalk Positions (국산 원료잎담배의 착엽위치에 따른 향기성분 및 휘발성 성분의 변화)

  • Hwang Keon- Jung;Rhee Moon-Soo;Kim Chung Ryul
    • Journal of the Korean Society of Tobacco Science
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    • v.27 no.1 s.53
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    • pp.127-133
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    • 2005
  • This study was conducted to determine the aroma and volatile component changes from a different stalk positions of Korean flue-cured tobacco. Eight different stalk positions of flue-cured leaf tobaccos harvested in 2001 were used for this study. Thermal extraction method at two different treatment temperature($50\;amp;\;80^{\circ}C$) was applied for this experiment. Forty eight kinds of aroma and volatile components such as 2,4-heptadienal, hexadecane, 1-methyl-1H- pyridine, 2,5-dimethyl-1H-pyrrole were analyzed by using thermal extraction method. All of aroma and volatile components of leaf tobaccos were changed from a different stalk positions and treatment temperature. Leaf tobaccos in middle stalk position have a higher concentration of aroma and volatile components such as norsolanidione, 4-pyridinecarboxaldehyde, 4-methyl-4-OH-2-pentanone, acetic acid, propylene glycol, 1-methyl-2-pyrrolidinone, 2,5-dimethyl-1H-pyrrole. Also, Megastigmatrienone 1, 3-oxo-[alpha]­ionol, 6,10,14-trimethyl-2-pentadecanone, heptadecane, 6-methyl-2-isohexyl-l-heptene concentration were low in the middle stalk position and high in both bottom and upper position. Treatment temperature affected on the changes of many aroma and volatile components in leaf tobacco. Most of aroma and volatile components such as, 2,4-Heptadienal, dodecanoic methylester, famesol isomer and 3-acetylpyridine were sharply increased as increasing treatment temperature. This results can be used to estimate the aroma characteristics of cigarette blend using a different stalk position of leaf tobacco.

Bioequivalence of Pinatos Capsule 10 mg to Ketas Capsule 10 mg (Ibudilast 10 mg) (케타스 캡슐 10밀리그램(이부딜라스트 10 밀리그램)에 대한 피나토스 캡슐 10밀리그램의 생물학적동등성)

  • Kang, Hyun-Ah;Kim, Se-Mi;Kang, Min-Sun;Yoo, Dong-Jin;Lee, Sang-No;Kwon, In-Ho;Yoo, Hee-Doo;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.40 no.2
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    • pp.117-123
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    • 2010
  • Ibudilast, 3-isobutyryl-2-isopropyrazolo[1,5-a]pyridine, is a nonselective inhibitor of cyclic nucleotide phosphodiesterase (PDE). It preferentially inhibits PDE 3A, PDE4, PDE10 and PDE11 as well as a number of the other PDE families, albeit to a lesser extent. Ibudilast is used clinically to treat bronchial asthma and cerebrovascular disorders. Thes e clinical uses are based on the ability of ibudilast to inhibit platelet aggregation, improve cerebral blood flow and attenuate allergic reactions. The purpose of the present study was to evaluate the bioequivalence of two ibudilast capsules, Ketas capsule (Handok Pharmaceuticals Co., Ltd.) and Pinatos capsule (Sam Chun Dang Pharm. Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The in vitro release of ibudilast from the two ibudilast formulations was tested using KP Apparatus method with various dissolution media. Twenty six healthy male subjects, 23.31${\pm}$1.09 years in age and 70.45${\pm}$8.51 kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After a single capsule containing 10 mg as ibudilast was orally administered, blood samples were taken at predetermined time intervals and the concentrations of ibudilast in serum were determined using HPLC/UV detector. The dissolution profiles of two formulations were similar in all tested dissolution media. The pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated, and computer programs (Equiv Test and K-BE Test 2002) were utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, Ketas, were 6.99%, -2.48% and 9.93% for $AUC_t$, $C_{max}$ and $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 (e.g., log 0.8791~log 1.1861 and log 0.8347~log 1.1199 for $AUC_t$ and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Pinatos capsule was bioequivalent to Ketas capsule.

Study on the Charge-Transfer Complexes Formed between the Derivatives of Nitrobenzene and Some Organic Solvent Molecules (용매성 유기분자와 니트로벤젠 및 그의 유도체와의 전하전이 착물에 관한 연구)

  • Doo-Soon Shin;Si-Joong Kim
    • Journal of the Korean Chemical Society
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    • v.17 no.2
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    • pp.85-94
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    • 1973
  • The stability constants of the charge-transfer complexes formed between three derivatives of nitrobenzene, i.e., 1,3,5-trinitrobenzene, m-dinitrobenzene, nitrobenzene and eleven organic molecules such as $\alpha-picoline$, pyridine, dimethylsulfoxide, N, N'-dimethylacetamide, tetrahydrofurane, 1, 4-dioxane, diethyl ether, acetonitrile, propylene oxide, epichlorohydrine, and methyl acetate, have been determined by ultraviolet absorption spectroscopy in carbon tetrachloride solution at 25.0$^{\circ}C$. The parameters of the electrostatic effect ($E_D$) and covalent effect ($C_D$) for the eleven organic compounds have been calculated from the modified equation of the double-scale enthalpy,$logK = E_AC_A+E_DC_D$ and also the shift of C=O vibrational frequency in infrared spectra for N,N'-dimethylacetamide have been measured from the solutions of above organic compounds. The empirical equation, ${\Delta}{\nu}_{C=O} = 37.4-5.47E_D+12.1C_D$, related to the parameters and the frequency shift has been derived. It seems that the stabilities of the complexes principally depend on the covalent effect. Especially it is found that $\pi$ orbitals in molecules, in addition to the parameters, play the important role in forming the charge-transfer complexes.

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Production of NAD from adenine and nicotinamide by Saccharomyces sake KBA No.6 (Saccharomyces sake KBA No. 6에 의한 adenine과 nicotinamide로부터 nicotinamide adenine dinucleotide(NAD)의 생산)

  • Choi, In-Girl;Hwang, Ki-Chul;Bang, Won-Gi
    • Applied Biological Chemistry
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    • v.35 no.3
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    • pp.157-164
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    • 1992
  • In order to produce nicotinamide adenine dinucleotide (NAD) which is a pyridine nucleotide coenzyme, Saccharomyces sake KBA No. 6 having high NAD content was selected from 12 strains of yeast and various factors affecting the production of NAD were investigated. For NAD production, 4% of glucose was effective as a carbon source and 2% of bactopeptone was the best nitrogen source. The optimum pH and temperature was 5.0 and $30^{\circ}$, respectively. Also, when 4 mg/ml of nicotinamide and 3 mg/ml adenine were used as precursors simultaneously, NAD production was the best. To increase NAD production, 2 valence metal ions were used during cultivation and $Zn^{2+}$ was very efficient. Among the surface active agents, anionic sodium dodesyl sulfate (SDS) was effective. Under the optimum conditions, the maximum amount of produced NhD was 35 mg/100 ml medium after cultivation of 144 hrs and 89% of total NAD amount, 31 mg of NAD, was leaked into culture broth.

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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
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    • v.15 no.2
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    • pp.132-138
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    • 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.

N-Terminal Sequences of ${\lambda}$-type Bence Jones Proteins (${\lambda}$형(型) Bence Jones 단백질(蛋白質)의 N 말단주변(末端周邊)의 아미노산배열순서(酸配刻順序)에 관한 연구(硏究))

  • Kim, Jun-Pyong
    • Applied Biological Chemistry
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    • v.13 no.1
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    • pp.65-72
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    • 1970
  • Two peptides (Im pr-M, Im ch-M) derived from Im ${\lambda}-type$ of Bence Jones Protein and one peptide (Ikch-M) from Ik were separated and purified using the Dowex $50{\times}2$ column $(1{\times}20\;cm)$ and Dowex $1{\times}2(0.9{\times}50\;cm)$. The buffer solution was composed of 1% pyridine and IM formic acid in Dowex $1{\times}2$ column. The blocked N-terminal was examined with ninhydrin reaction before and after alkaline hydrolysis, which was fractionated by Dowex $1{\times}2$ column. Pyrro-glutamic acid in N-terminal residue was identified by comparing with the authentic pyrro-glutamic acid through a high voltage electrophoresis (pH 3.5, 3000 V.) after the peptide Im pr-M (PCA. Ser) was cleavaged at the position of serine with cone. (12 N) HCl and the pyrro-glutamic acid was converted to glutamic acid by treating it with N-NaOH for 116 hours at $27^{\circ}C$. The substractive method was applied to find out the sequence of peptides and carboxypeptidase A was employed to release C-terminal residue from the peptide. In present study PCA. Ser in Im Pr-M was isolated from the pronase digested ${\lambda}$-type Bence Jones protein. The yield of the Im Pr-M was 79.6 percent of its theoretical value, based on the molecular weight of Bence Jones Protein. Im ch-M (PCA. Ser Val. Leu) was isolated from the chymotrypsin digested ${\lambda}$-type Bence Jones Protein. The yield of the Im ch-M was 72.2 percent. based on the molecular weight of Bence Jones Protein. Ik ch-M (PCA. Ser. Ala. Leu) was isolated from the chymotrypsin digested ${\lambda}$-type Bence Jones Protein and its yield was 42% based on the molecular weight of Bence Jones Protein.

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