• 제목/요약/키워드: Dioxane

검색결과 212건 처리시간 0.024초

Synthesis of 11-Deoxydaunomycinone and Novel 10-Fluoroanthracyclinone Derivatives

  • Rho, Young S.;최영희;김규일;신홍식;유동진;정채준;김선하
    • Bulletin of the Korean Chemical Society
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    • 제20권5호
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    • pp.551-555
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    • 1999
  • 11-Deoxydaunomycinone 15 and 10-fluoroanthracyclinone derivatives 9, 10 were obtained. Naphthalenone 4 prepared from 2-(2,4-pentadienyl)-1,3-dioxane 2 with methyl vinyl ketone and hydrolysis with HClO4 was condensed with phthalidesulfone 5 through Michael type reaction, and was converted to 7 by epoxidation. Epoxide 7 was transformed to trione 12 using reduction-oxidation or hydrofluorination process, and then to 15 by introducing several functional groups. Compound 8 obtained in the course of the reaction of epoxide 7 and HF/ Pyr was used for the synthesis of compounds 9, 10.

Ruthenium Catalyzed Synthesis of 1-Substituted Perhydroazocines from Primary Amines and 1,7-Heptanediol

  • Shim, Sang-Chul;Doh, Chil-Hoon;Yoon, Jeum-Ho;Lee, Dong-Yub;Youn, Young-Zoo
    • Bulletin of the Korean Chemical Society
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    • 제12권6호
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    • pp.649-652
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    • 1991
  • The reaction of primary aromatic amines with 1,7-heptanediol in the presence of a catalytic amount of ruthenium complex in dioxane at $180^{\circ}C$ for 24 hours gave the corresponding 1-substituted perhydroazocines in moderate yield.

Electronic excitation energy quenching of PPD by $CCl_4$ in different solvents

  • Biradar, D.S.;Thipperudrappa, J.;Hanagodimath, S.M.
    • Journal of Photoscience
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    • 제12권1호
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    • pp.51-54
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    • 2005
  • The electronic excitationenergy quenching of 2, 5-diphenyl-1, 3, 4-oxadiazole (PPD) by Carbon tetrachloride ($CCl_4$) in different solvents viz, n-hexane, n-heptane, toluene, benzene, cyclohexane, 1, 4- dioxane has been carried out at room temperature to understand the role of quenching mechanism. The Stern-Volmer plots have been found to be linear. As probability of quenching per encounter 'p' is less than unity, and the activation energy for quenching '$E_a$' is greater than the activation energy of diffusion '$E_d$', it is inferred that the fluorescence quenching mechanism is not due to material diffusion alone.

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산성용액 중에서 Phenyl N-(p-chlorobenzoyl)chloroformimidate 유도체의 가수분해 반응 메카니즘 (Mechanism of the Hydrolysis of Phenyl N-(p-chlorobenzoyl)Chloroformimidate Derivatives in Acid Media)

  • 성낙도;전용구;권기성;김태린
    • 대한화학회지
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    • 제31권4호
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    • pp.352-358
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    • 1987
  • $25^{\circ}C$의 1 : 4 dioxane-물의 혼합용액속에서 파라-치환된 phenyl N-(p-chlorobenzoyl)chloroformimidate (I) 유도체들의 가수분해 반응속도 상수를 측정하고 반응속도식, 치환기 효과$(\rho\>{\rho}^+)$, 생성물 분석 및 분자궤도 함수의 계산 결과로부터 pH3.0 이하에서는 azocarbonium 이온(II)이 생성되는 $S_N1$반응 메카니즘으로 무촉매 반응이 일어나며, pH 4.0이상에서는 전이상태(III)를 지나는 $S_N2$반응 메카니즘을 통하여 염기 촉매반응이 일어남을 제안 할 수 있었다. 4가지 peri planar형태 이성질체들의 상대적인 안정도는 각각 (E-ap) > (Z-ap) > (E-sp) > 및 (Z-ap)이었고, (E-ap)형태의 가장 안정한 입체구조는 benzimidochloroformyl group면에 대하여 Y-치환 phenyl group이 수직$(90^{\circ})$을 이루었으며 (I)의 활성화된 azomethine탄소 원자에 대하여 물분자는 시그마 공격에 의하여 친핵성 반응이 일어난다.

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Benzohydrazonyl Bromide의 加水分解 反應메카니즘에 관한 反應速度論的 硏究 (Kinetic Studies on the Mechanism of Hydrolysis of Benzohydrazonyl Bromide)

  • 권기성;김태린
    • 대한화학회지
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    • 제20권3호
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    • pp.221-228
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    • 1976
  • $60{\%}$ dioxane 수용액에서 hydrazonyl bromide의 여러 유도체$(p-H,\;p-CH_3,\;p-OCH_3,\;p-Br,\;p-Cl\;및\;p-NO_2)$의 pH에 따르는 가수분해 반응속도를 $25^{\circ}C$에서 자외선 분광광도법으로 측정하여 넓은 pH 범위에서 잘 맞는 반응속도식을 구하였다. 가수분해 반응속도에 미치는 치한기효과를 검토하기 위하여 Hammett plot한 결과 pH 2 이하에서는 ${\Phi}$ = -0. 94, pH 4 이상에서는 ${\rho}$ = 0.54을 얻었다. pH에 따르는 반응속도 상수의 변화에 미치는 용매효과 브롬음이온효과 및 치환기효과등으로 부터 hydrazonyl bromide의 가수분해는 pH 2 이하에서는 carbonium ion 중간체를 거쳐 반응이 진행되는 $S_N1$ pH 4 이상에서는 hydrazonyl bromide에 직접 hydroxide ion이 반응하는 이른바 $S_N2$반응이 그리고 pH 2와 pH 4 사이에서는 이 두반응이 경쟁적으로 일어남을 알 수 있었다.

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졸-겔법에 의한 mullite합성시 건조 첨가제가 건조 및 소성에 미치는 영향 (Effects of Drying Agents on the Drying and Calcination in Synthesis of Mullite by Sol-Gel Process)

  • 함영민;홍영호;최승일
    • 공업화학
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    • 제4권3호
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    • pp.497-504
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    • 1993
  • 본 연구는 고온 구조재료 및 전자재료로 주목받고 있는 복합산화물인 mullite($3Al_2O_3${\cdot}2SiO_2$)를 금속알콕사이드에 의한 졸-겔법으로 합성함에 있어서 재활용품으로서의 aluminium foil을 aluminium 금속원으로 사용하여 알루미늄 알콕사이드를 제조하고 $Si(OC_2H_5)_4$와 혼합하여 가수분해 단계에서 건조조절화학첨가제(Drying Control Chemical Additives, DCCA)를 첨가함으로써 건조시간을 단축시키려는 시도를 하였으며 이러한 DCCA가 mullite 물성에 어떠한 영향을 주는지 검토하고자 하였다. 이때 DCCA로 N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane과 Oxalic acid가 첨가되었으며 건조된 겔을 각 온도별로 소성하여 TG-DTA, FT-IR, XRD 및 SEM을 사용하여 결정의 전이과정 및 각 소성온도에서의 결정상태 등을 관찰하였다. DCCA를 첨가하여 건조시킨 결과 0.1mole의 DMF를 첨가하였을 경우 DCCA를 첨가하지 않았을 때보다 건조시간이 1/2 정도 단축되었으며 분석결과 mullite의 결정형성에 큰 영향을 미치지 않았음을 확인하였다.

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Poly(ethylene 2,6-naphthalate) 필름의 연신에 따른 동적 점탄성 거동 해석 (Analysis of Dynamic Viscoelasticity Behavior on Drawing of Poly(ethylene 2,6-naphthalate) Film)

  • 강영아;김경효;조현혹
    • 한국염색가공학회지
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    • 제11권5호
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    • pp.44-54
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    • 1999
  • Poly(ethylene 2,6-naphthalate), PEN, is a relatively well-known polymer used for engineering purposes. Naphthalene ring provides rigidity to the polymer backbone, thus, it elevated the glass transition temperature and enhanced mechanical properties. The structure and properties of PEN affect a processing conditions severely, and the high-thermal stability have been had a poor thermal processibility. Hence, the basic mechanism of solvent drawing, is very much the same as that of thermal drawing from glassy state since both involve the inducement of segmental mobility. The former achieves the goal by use of chemical energy, and the latter does so by use of thermal energy. Generally, the sorption of the solvent by the polymer has a plasticizing effect, and leads to a lowering of the glass transition temperature, $T_g$. In this paper, the dynamic viscoelasticity behavior in liquid-drawing process of an unoriented amorphous PEN films were investigated using Rheovibron. The results are as follows : (1) For the drawing in silicone oil, the drawing below $T_g$. had $\alpha{2}$-dispersion due to an inhomogeneous taut structure. (2) For the drawing in water, the inhomogeneous taut structure reduced by the effect of plasticization even below $T_g$. (3) For the drawing in butanol, the only aliphatic segment in PEN have some molecular mobility but the mobility of the aromatic segment having naphthalene ring is nearly impossible. (4) For the drawing in dioxane/water mixing solvent, the solvent effect is complementary each other and accordingly the entire molecular conformation have stable state. (5) For the drawing in dioxane/butanol mixing solvent, the inhomogeneity of the taut structure and the aromatic segment increase with increasing the temperature and this tendencies correspond with that of the draw ratio.

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o-Chlorobenzylidenemalononitrile의 가수분해 및 분석에 관한 연구 (A Study on the Hydrolysis and Analysis of o-Chlorobezylidenemalononitrile)

  • 박성우;김남이;김동환;홍성욱;성낙도;김일광;오인교
    • 분석과학
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    • 제5권4호
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    • pp.443-454
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    • 1992
  • o-Chlorobenzylidenemalononitrile(CS), chloroacetophenone 및 bromophenylacetonitrile의 이성질체와 같은 최루 자극성 물질들의 가수분해, 산화, 환원, 열분해 및 대사에 의한 화합물의 분석은 법과학적 측면에서 주요한 의미가 있다. 본 실험에서는 10% MeOH-$H_2O$ 및 10% dioxane-$H_2O$ 용액에서 pH 1.0~11.0과 온도 변화에 따른 CS의 가수분해 조건을 검토하고 가수분해 생성물이 o-chlorobenzaldehyde와 malononitrile임을 분광학적 방법 및 전기화학적 방법에 의해 확인하였다.

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1,3-디옥산을 함유한 분해성 계면활성제의 합성의 및 계면 특성 (Synthesis of Surface Active Properties of Destructible Surfactants with 1,3-Dioxane)

  • 김치회;노윤찬;김유옥;남기대
    • 한국응용과학기술학회지
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    • 제13권3호
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    • pp.61-71
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    • 1996
  • In acid-catalyzed acetal cyclization of long aliphatic aldehydes($R=n-C_7H_{15}$ ; $n-C_9H_{19}$ ; $n-C_{11}H_{23}$) with 1,1,1-tris(hydroxymethyl)propane, 2-alkyl-5-hydroxymethyl-5-ethyl-1,3-dioxanes were obtained. The final products, sodium 2-alkyl-5-(sulfonatedpropylethermethyl)-5-ethyl-1,3-propanesultion in the presence of sodium hydride. These compounds were a new group of destructible surfactants which were readily hydrolyzed and oxidized in natural water reservoirs. Physical properties of these new compounds involved some surface properties such as Krafft point(Kp), critical micelle concentration(cmc), surface tension of aqueous solutions near cmc(${\gamma}_{min}$), foaming power, emulsion power and hydrolysis properties were determined. The destructible surfactants containing 1,3-dioxane ring were synthesized to about $85{\pm}5.5%$ yield. The cmc values of the compounds by ring method were assumed to $0.5{\sim}5.0{\times}10^{-3}mol/L$ range and surface tensions at cmc were $29.5{\sim}33.0dyne/cm$ respectively at $25^{\circ}C$. The foaming power and foam stability were $170{\sim}230mm$ and $52{\sim}135mm$ respectively at $1{\times}10^{-2}mol/L$, foam was occurred rarely below $1{\times}10^{-3}mol/L$. The emulsion property of liquid paraffin was better than that of soybean oil. For hydrolysis property with ph and time, these compounds were decomposed within about 200minutes at $ph1{\sim}2$. Hopefully these compounds are expected to be a good O/W emulsifier that have decomposability in acid and may be used in the process which do not need foaming.