• 제목/요약/키워드: good solvent condition

검색결과 58건 처리시간 0.021초

TMEDA: Efficient and Mild Catalyst for the Acylation of Alcohols, Phenols and Thiols under Solvent-free Condition

  • Kadam, Santosh T.;Lee, Han-Bin;Kim, Sung-Soo
    • Bulletin of the Korean Chemical Society
    • /
    • 제30권5호
    • /
    • pp.1071-1076
    • /
    • 2009
  • N,N,N′,N′-tetramethylethylenediamine (TMEDA) acts as a simple, mild and efficient catalyst for the acylation of alcohols, phenols and thiols at room temperature under solvent-free condition. Acylation reaction with acetic anhydride and benzoic anhydride proceeds with good to excellent yield in the presence of TMEDA as the catalyst.

유동성이 우수한 분체특성을 갖는 세파졸린 나트륨 진공동결건조 분말의 제조 (Preparation of Freeze-dried Cefazolin Sodium Bulk Powder with Good Flowability)

  • 조정식;정은주
    • 약학회지
    • /
    • 제42권3호
    • /
    • pp.284-289
    • /
    • 1998
  • The effect of reaction condition, solvent addition and thermal treatment on the bulk density, crystallinity and chemical properties of the freeze-dried cefazohn sodium was inves tigated to prepare the cefazolin sodium powder for injection with good flowability. Crystalline cefazolin sodium powder with high untapped-bulk density (about 45%) and low compressibility (about 40%) was obtained by solvent addition to the very highly concentrated cefazohn sodium solution followed by subsequent thermal treatment before freeze-drying. The desirable solvent was low substituted alcohol such as isopropyl alcohol and anhydrous ethanol with the final concentration of about 9%. The pH adjustment and nitrogen gas purging during the reaction did not give significant effect on the chemical properties such as content, color, transmittance and pH of the reconstituted cefazolin sodium aqueous solution.

  • PDF

Temperature-dependent Conformational changes of Single Polymer Chains

  • Ohno, Naoto;Watanabe, Kenji;Nakajima, Ken;Nishi, Toshio
    • 한국고분자학회:학술대회논문집
    • /
    • 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
    • /
    • pp.342-342
    • /
    • 2006
  • Atomic force microscope (AFM) enables us to stretch a single polymer chain by picking it at its two modified termini. Using this method called "nanofishing," we have studied statistical properties of single polymer chains. A force-extention curve obtained for a polystyrene with thiol termini in a cyclohexane showed a good agreement with a worm-like chain (WLC) model, and thus gave microscopic information about entropic elasticity. In this report, the experiments were performed at wide-range temperatures, resulting in wide-range solvent qualities from poor to good solvent condition. The temperature dependence of statistical properties of polystyrene was examined. The coil-strand transformation realized in a poor solvent was also discussed.

  • PDF

Microwave-Assisted One-Pot Synthesis of Octahydroquinazolinone Derivatives Catalyzed by Thiamine Hydrochloride Under Solvent-free Condition

  • Badadhe, Pravin V.;Chate, Asha V.;Hingane, Dattatraya G.;Mahajan, Pravin S.;Chavhan, Namdev M.;Gill, Charansingh H.
    • 대한화학회지
    • /
    • 제55권6호
    • /
    • pp.936-939
    • /
    • 2011
  • Thiamine hydrochloride (VB1) has been used as an acid catalyst in organic synthesis. One pot three component Biginelli condensation of dimedone, urea/thiourea and substituted aromatic aldehydes catalyzed by 10 mol % of thiamine hydrochloride (VB1) in solvent free condition under microwave irradiation in good to excellent yields has been investigated. Utilization of microwave irradiation, simple reaction conditions, short reaction time, ease of product isolation, and purification makes this manipulation very interesting from an economic and environmental perspective.

미소 수용 Cyclohexange 중에서 분말 Lipase에 의한 분자내 에스테르화반응 (Intramolecular Esterification by Lipase Powder in Microaqueous Cycohexane)

  • 이민규;감삼규
    • 생명과학회지
    • /
    • 제5권4호
    • /
    • pp.155-161
    • /
    • 1995
  • The effects of substrate concentration, enzyme concentration, reaction temperature, and water content were investigated in intramolecular esterification. This study used cyclohexane as organic solvent, power lipase as enzyme, and benzyl alcohol and octanoic acid as substrate. The initial reaction rate was found to be proportional to enzyme concentration; followed Michaelis-Menten equation for octanoic acid; and was inhibited by benzyl alcohol . The observed initial reaction rate first increased, then decreased with increasing reaction temperature, giving rise to the maximum rate at 20$\circ$. The drop in the reaction rate at higher temperature was to partition equilibrium change of substrate between organic solvent and hydration layer of enzyme molecule in addition to the deactivation by enzyme denaturation. Water layer surrounding enzyme molecule seemed to activate in organic solvent and the realistic reaction was done in the water layer. In the enzymatic reaction in organic solvent, the initial reaction rate was influenced by partition quilibrium of substrate, so the optimum condition of substrate concentration, enzyme concentration, reaction temperature, and water content would give a good design tool.

  • PDF

Studies on Solvent Extraction and Flotation Technique Using Metal-Dithizone Complexes(II). Determination of Trace Elements in Water Samples by Solvent Sublation

  • 김영상;최윤석;최희선
    • Bulletin of the Korean Chemical Society
    • /
    • 제19권10호
    • /
    • pp.1036-1042
    • /
    • 1998
  • The preconcentration and determination of trace elements in water samples were studied by a solvent sublation utilizing dithizonate complexation. After metal dithizonates were formed, trace amounts of cadmium, cobalt, copper and lead were floated and extracted into small volume of a water-immiscible organic solvent on the surface of sample solution and determined in the solvent directly by GF-AAS. Several experimental conditions as formation condition of metal-dithizonate complexes, pH of solution, amount of dithizone, stirring time, the type and amount of surfactants, N2 bubbling rate and so on were optimized for the complete formation and effective flotation of the complexes. And also four kinds of light solvents were compared each other to extract the floated complexes, effectively. After the pH was adjusted to 4.0 with 5 M HNO3, 8.0 mL of 0.05% acetone solution of dithizone was added to 1.00 L water sample. The dithizonate complexes were flotated and extracted into the upper methyl isobutylketone (MIBK) layer by the addition of 2.0 mL 0.2% ethanolic sodium lauryl sulfate solution and with the aid of small nitrogen gas bubbles. And this solvent sublation method was applied to the analysis of real water samples and good results of more than 85% recoveries were obtained in spiked samples.

Analytical Method for Dioxin and Organo-Chlorinated Compounds: (Ⅱ) Comparison and Extraction Methods of Dioxins from XAD-2 Adsorbent

  • 양정수;이성광;박영훈;이대운
    • Bulletin of the Korean Chemical Society
    • /
    • 제20권6호
    • /
    • pp.689-695
    • /
    • 1999
  • Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

GC-MS를 이용한 식물홀몬 분석 (Analysis of Plant Hormones using GC-MS)

  • 조광연
    • 한국작물학회지
    • /
    • 제34권s01호
    • /
    • pp.26-32
    • /
    • 1989
  • The analytic principles of GC and MS were explained in relation to plant hormone analyses and the characteristics of two instruments were compared. The selection of column, condition of measurement and the method of ionization to get a good spectrum were also briefly described. Finally, the pre-treatment of sample by solvent extraction method to remove the unnecessary part of sample and the synthetic method, especially reagents and reaction condition, for the preparation of ether or ester derivative which can be easily vaporized in GC were explained.

  • PDF

NaHSO4/SiO2: Solvent-Free 반응 조건에서 β-Enaminone들과 2-Methylquinolin-4(1H)-One들의 합성을 위한 효율적인 촉매 (NaHSO4/SiO2: An Efficient Catalyst for the Synthesis of β-Enaminones and 2-Methylquinolin-4(1H)-Ones under Solvent-Free Condition)

  • Sapkal, Suryakant B.;Shelke, Kiran F.;Shingate, Bapurao B.;Shingare, Murlidhar S.
    • 대한화학회지
    • /
    • 제54권6호
    • /
    • pp.723-726
    • /
    • 2010
  • 마이크로 반응을 이용하여 $NaHSO_4/SiO_2$을 촉매로 하는 solvent-free 합성을 통하여 $\beta$-enaminone 과 2-methylquinolin-4(1H)-one 및 그 유도체를 합성하는 효율적인 방법을 개발하였다. 반응 시간이 짧고, 수율이 좋았으며, 마이크로웨이브를 사용하지 않는 반응보다는 높은 선택성, 간단성, 무용매 반응 및 친환경적인 반응이다.

자색고구마 Anthocyanin 색소의 추출조건 결정 (Determination of the Conditions for Anthocyanin Extraction from Purple-Flashed Sweet Potato)

  • 이장욱;이향희;임종환;조재선
    • 한국식품영양과학회지
    • /
    • 제29권5호
    • /
    • pp.790-795
    • /
    • 2000
  • To establish the optimum conditions for the extraction of anthocyanin pigment from purple-fleshed sweet potato, a suitable extraction solvent with the optimum citric acid concentration for acidification of the solvent, and the optimum extraction time and temperature were determined. Twenty percent ethanol solution acidified with citric acid was found to be a good solvent for the extraction of the pigment from purple-fleshed sweet potato. About 10 hour extraction at room temperature was appropriate for the extraction. pH of the extract was below 3 when more than 0.7% citric acid was added. The higher the concentration of citric acid added was, the higher the total optical density (TOD) of the extract was. However, the increase in TOD of the extract was insignificant when more than 1% of citric acid was added. Therefore, addition of 1% citric acid was determined for acidification of the extracting solvent. Though the initial rate of the pigment extraction increased as the extracting temperature increased, extraction at higher temperatures of 60 or 8$0^{\circ}C$ for an extended time caused a decrease in the extraction yield due to degradation of the pigment. The optimum extraction temperature for the anthocyanin pigment from purple-fleshed sweet potato with the solvent used was determined as 4$0^{\circ}C$.

  • PDF