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提出了一条方便地制备5-芳基-3,5-二乙氧基-2(5H)-呋喃酮化合物的合成路线,并对合成路线的反应机理进行了研究。应用设计的路线,合成了一组新颖的高度官能团化的2(5H)-呋喃酮化合物,所有化合物的结构均经过元素分析或高分辨率质谱,IR,NMR和MS确证。 相似文献
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手性3-溴-2(5H)-呋喃酮的合成及其串联的不对称Michael加成 反应的研究 总被引:2,自引:0,他引:2
研究了新的手性试剂,5-(l-孟氧基)-3-溴-呋喃酮(5a)的合成及其与亲核性醇发生的串联不对称双Michael加成/分子内亲取代反应。通过此反应,一举生成了四个新的手性中心,得到了一般方法难以合成的含有多个手性中心的丁内酯并螺-环丙烷类化合物8a~8d。详细报道了8a~8d的合成方法以及它们的[α]、IR、UV、^1^HNMR、^13^CNMR、MS、元素分析等结构分析数据。此不对称双Michael加成/分子内亲核取代反应可以为某些新的光学活性螺-环内丙烷类化合物以及某些复杂结构的分子提供合成策略。 相似文献
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Reaction of phenylnitromethane with acetic anhydride/sodium acetate at 80–85° produces N-benzoyl-N,O-diacetylhydroxylamine, which can be isolated in 30% yield. This compound was proposed previously as an intermediate in a similar reaction which had yielded only benzoic anhydride, triacetylhydroxylamine and acetanilide. 相似文献
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Xizhen Zhu Kevin D. Kreutter Huaping Hu Mark R. Player Micheal D. Gaul 《Tetrahedron letters》2008,49(5):832-834
A novel reagent combination, Tf2O/Na2CO3·1.5H2O2, has been developed for the oxidation of highly electron deficient pyridines to their corresponding N-oxides. The N-oxidation reaction, utilizing the in situ generated peracid, proceeds under mild conditions that allow for a number of functional groups and substitution patterns on the pyridine ring. 相似文献
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Oxidation of primary nitroalkanes by acetic anhydride/sodium acetate has been found to be more complex than previously suspected. Phenylnitromethane, with acetic anhydride/sodium acetate at 60–80°, for example, gives a mixture of benzoic anhydride, triacethylhydroxylamine and acetanilide, through the mixed anhydride as a key intermediate. Evidence in support of this latter species has been obtained by carrying out the oxidation in the presence of dimethyl acetylenedicarboxylate as a 1,3-dipolarophile, when 3-phenyl-4,5-dicarbomethoxyisoxazole is formed in 82% yield. A number of other 3-alkyl- and 3-aryl-4,5-dicarbomethoxyisoxazoles have been prepared in a similar manner. 相似文献
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In this paper, a novel and precise analytical procedure has been developed for quantitative determination of sodium percarbonate (SPC) in washing powder. The method is based on the partial least squares (PLS) treatment of data obtained by attenuated total reflectance Fourier transform infrared (ATR FT-IR) spectrometry in wavenumber region of 1435-1342 cm−1. The statistical parameters such as R2, RSD, SEC and SECV have been evaluated, and number of factors, number of scan and the resolution have been optimized. In this method R2 and RSD for five independent analyses of a 0.552 g per 100 g solution of SPC, SEC for 10 standard samples and SECV for five validation samples were 0.998, 1.011, 0.002 and 0.039 respectively.Results obtained for six different commercial washing powders compared well with those obtained with a standard method. 相似文献
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The reaction of acetic [13C]formic anhydride with sodiumpentacarbonylmanganate proceeds rapidly at 0°C to give 13CO substituted pentacarbonylmanganese hydride as the predominant product. The results are consistent with the formation of a short-lived neutral formyl complex, (CO)5Mn13CHO. 相似文献
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Philippe Marchal Gatane Coppens Roger Legras Jean-Marc Dekoninck 《Journal of polymer science. Part A, Polymer chemistry》1995,33(5):757-766
Polyamide 6 (PA6) and poly(metaxylene adipamide) (PAmXD6) were blended in a batch mixer with anhydrides such as phthalic anhydride, n-octadecyl succinic anhydride, and anhydride-grafted ethylene propylene rubber. The melt viscosity, the solution viscosity, and chain end concentration were studied during the mixing. PA was first mixed 5 min to get an homogeneous melt prior to the anhydride addition. The introduction of the anhydride to the molten polyamide resulted in large decreases of melt and solution viscosities and of amine chain end concentrations. The anhydride units react with amine chain ends to form imide groups. The resulting low amine chain end concentration causes hydrolysis reaction to maintain the condensation equilibrium. As a consequence an increased carboxylic chain end concentration is observed. The imide concentration was studied by IR. It was shown that when most of the amine chain ends are consumed, the remaining anhydride reacts with amino groups formed by polyamide hydrolysis. © 1995 John Wiley & Sons, Inc. 相似文献
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采用分光光度法研究了电子给体苯巴比妥钠与π电子受体茜素红的荷移反应,建立了荷移分光光度法测定苯巴比妥钠的方法。在水溶液中,苯巴比妥钠与茜素红荷移络合物的最大吸收波长为530 nm,该络合物的组成为1∶1,表观摩尔吸光系数ε为4.43×103L.mol-1.cm-1,稳定常数为2.30×105。药物质量浓度在5~40 mg/L范围内符合比尔定律,相关系数为0.9996。当苯巴比妥钠浓度为20 mg/L时,10次测定结果的相对标准偏差为1.3%。测定了针剂中的苯巴比妥钠,加标回收率在98.9%~105%之间。 相似文献
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Summary The bicyclic acetate obtained in the reaction of 2-pinene oxide with acetic anhydride is a mixture of (–)-and (±)-trans-pinocarveol acetates; one of the monocyclic acetates obtained is a mixture of (+) and (±)-trans-carveol acetates.Translated from Izvestiya Akademii Nauk SSSR, Khimicheskaya, No. 12, pp. 2144–2152, December, 1965 相似文献
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Under the conditions of the Polonovsky reaction, N-(2,7-dimethyl-2,7-octadienyl)-N,N-dimethylamine oxide gives 2,7-dimethyl-2,7-octadienal and N-(2,7-dimethyl-2,7-octadienyl)-N-methylacetamide. Under the same conditions, N-(2,7-dimethyl-2,7-octadienyl)-N,N-dietnylamine oxide dihydrate does not undergo the Polonovsky reaction and gives the rearrangement product, O-(1-isopropenyl-5-methyl-5-hexenyl)-N,N-diethylhydroxylamine, and the hydration product, O-[1-(1-hydroxy-1-methyl)ethyi-5-methyl-5-hexenyl]-N,N-diethylhydroxylamine.The work was accomplished under the financial support of the Russian Fund for the Fundamental Research (93-03-4219).Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1588–1590, September, 1993. 相似文献