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Zusammenfassung -Äthyl--phenylacetessigester (I) wurde bromiert, der resultierende -Bromacetylphenylbuttersäureester (II) mit NaBH4 zum Bromhydrin (III) reduziert. Umsetzung mit KCN lieferte den -Cyan--hydroxy--phenyl--äthylbuttersäureester (IV), der in Gegenwart vonRaney-Ni zu den beiden stereoisomeren 3-Äthyl-3-phenyl-4-hydroxypiperidonen-(2) (Va) und (Vb) reduziert wurde. Oxydation von (Vb) mit CrO3 lieferte das 3-Äthyl-3-phenylpiperidindion-(2,4) (VI).  相似文献   

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A one pot synthetic approach to the novel pyrazolyl, isoxazolyl and 1,2,3-(triazolyl)methyl-1,5-benzodiazepine system, by 1,3-dipolar cycloaddition of nitrilimines, benzonitriloxides and benzylazide to 1-propargyl-4-phenyl-1,5-benzodiazepin-2-one, is described. The structures of the obtained adducts have been assigned by means of spectroscopic measurements.  相似文献   

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The title compound cis-1,2-dicyano-1,2-bis(2-methyl-4-bromo-3-thienyl)ethane has been synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data: triclinic, space group P1^1, Z = 2, C14H8Br2N2S2, Mr = 428.16, a = 6.9410(5), b = 11.0150(9), c = 11.1760(8) A, α = 70.3390(10),β = 76.1860(10), γ = 79.5490(10)°, V= 776.59(10) A^3, Dc = 1.831 g/cm^3, μ(MoKα) = 5.478 mm^-1, F(000) = 416, R = 0.0487 and wR = 0.1453 for 2456 observed reflections with I 〉 2σ(/). X-ray analysis reveals that the two thiophene rings are significantly twisted with an average dihedral angle of 57.45°. The molecule adopts a photo-active antiparaUel conformation and the distance between the two reactive C atoms of thiophene rings is 3.465(8)A. These structural elements which exhibit a suitable geometry are extensively explored for photochromic behavior in the crystalline state.  相似文献   

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《Comptes Rendus Chimie》2002,5(6-7):517-523
Condensation of 4-hydroxy-6-methyl pyran-2-one 2 with 3-amino-1,2,4-triazole 1 in refluxing alcohol afforded 5-alkoxycarbonylmethyl-7-methyl-1,2,4-triazolo〚1,5-a〛pyrimidines and their isomers 5-alkoxycarbonylmethyl-7-methyl-1,2,4-triazolo〚4,3,-a〛pyrimidines 4. Reaction of hydrazine hydrate with compounds 4 and 5 yielded the corresponding hydrazid acids 6 and 7. Condensation of o-phenylenediamines 8 with esters 3(4) in refluxing xylol or with hydrazid acid 6(7) by melting reagents afforded 7(5)-〚benzimidazol-2-yl〛methyl-5(7)methyl-1,2,4-triazolo〚1,5-a〛(〚4,3-a〛)pyrimidines 9(10). The structures of the annealed compounds have been elucidated by their 1H, 13C NMR and Mass Spectroscopy data.  相似文献   

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Condensation of 3-amino-5-hydroxypyrazole 1 with triacetic acid lactone 2 in refluxed alcohols afforded 2-hydroxy-5,7-dimethylpyrazolo〚1,5-a〛pyrimidine 3 beside to 7-alkoxycarbonylmethyl-2-hydroxy-5- methylpyrazolo〚1,5-a〛pyrimidine 4. Action of hydrazine on compounds 4 yielded 7-hydrazinocarbonylmethyl-2-hydroxy-5-methylpyrazolo〚1,5-a〛pyrimidine 5. Condensation of o-phenylenediamines 6 with hydrazide 5 to melting reactants afforded 2-hydroxy-7-〚benzimidazol-2-yl〛methyl-5-methylpyrazolo〚1,5-a〛pyrimidines 7. Structures of the obtained products have been assigned by means of spectroscopic measurements.  相似文献   

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洪琳  陈莉雅  杨克 《化学学报》1989,47(5):509-511
本文研究了1-氯-3-硝基-2-丁烯与2-硝基丙烷钠盐的SRN1反应, 结果表明这种开链状纯脂肪族烯丙基型化合物发生了不重排的SRN1反应.  相似文献   

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徐丹  董学亮  刘明  余学军 《化学研究》2005,16(3):78-79,83
以过氧化氢为氧化剂,在碱性条件下氧化2-亚硝基-1-萘酚合成了2-硝基-1-萘酚,优化了反应条件,改进了分离方法,产品收率达到70%以上.  相似文献   

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The solubility of oxygen has been measured in a number of electrolytes [(LiCl, KCl, RbCl, CsCl, NaF, NaBr, NaI, NaNO3, KBr, KI, KNO3, CaCl2, SrCl2, BaCl2, Li2SO4, K2SO4, Mn(NO3)3)] as a function of concentration at 25°C. The solubilities, mol (kg-H2O)–1, have been fitted to a function of the molality m (standard deviation < 3mol-kg–1)
where A and B are adjustable parameters and the activity coefficient of oxygen )O2) = [O2]0/[O2]. The limiting salting coefficient, k S = (ln / m)m=0 = A, was determined for all salts. The salting coefficients for the chlorides and sodium salts showed a near linear correlation with the crystal molar volume V cryst = 2.52 r 3. The salting coefficients determined from the Scaled Particle Theory were in reasonable agreement with the measured values. The activity coefficients of oxygen in the solutions have been interpreted using the Pitzer equation
where is a parameter that accounts for the interaction of O2 with cations (c) and anions (a) with molalities m a and m c, and accounts for interactions for O2 with the cation and anion pair (c-a). The and coefficients determined for the most of the ions are in reasonable agreement with the tabulations of Clegg and Brimblecombe. The values of for most of the ions are a linear function of the electrostriction molar volume (Velect = V0V cryst).  相似文献   

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A number of efficient catalytic procedures for the oxidation of acid-sensitive substrate such as 2-methyl-3-buten-2-ol to the corresponding ketone (2-methylbutan-2-ol-3-one) are compared. Reaction with dioxygen (or quinone) and a palladium precursor (PdCl2 or [PdCl(NO2)(CH3CN)2]) under mild conditions (⋍ 35°C), gave good conversions (⋍ 98%) and good selectivities (⋍ 90%).  相似文献   

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Condensation of 2-methyl-1-pyrroline with chloroacetone or 3-chloro-2-butanone using LDA in THF afforded novel 2-(3-hydroxy-2-methyl-1-alkenyl)-1-pyrrolines via a peculiar reaction mechanism instead of the anticipated 2-(3-oxobutyl)-1-pyrrolines. The intermediacy of 2-(2,3-epoxy-2-methylalkyl)-1-pyrrolines in the latter transformation was demonstrated by immediate reductive epoxide ring opening utilizing lithium aluminium hydride in diethyl ether. Furthermore, 2-(3-oxobutyl)-1-pyrroline was prepared via an alternative approach through alkylation of 2-methyl-1-pyrroline with 3-chloro-2-(methoxymethyloxy)-1-propene using LDA in THF, followed by acid hydrolysis. Reduction of 2-(3-oxobutyl)-1-pyrroline by sodium borohydride in methanol afforded the corresponding 2-(3-hydroxybutyl)-1-pyrroline in good yield.  相似文献   

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