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以2-萘酚和80%水合肼为起始原料,经3步反应合成了光学活性的2,2'-二胺-1,1'-联萘。在缚酸剂存在下,将所得光学活性的二胺与甲基丙烯酰氯反应制备得到目标产物(R)-2,2'-二甲基丙烯酰胺-1,1'-联萘。各步产物的结构经核磁分析得到确认。研究了水合肼与2-萘酚的投料比对中间体2-萘肼收率的影响,以及缚酸剂类别、反应温度对目标产物收率的影响,得到了一种适宜的合成工艺路线。 相似文献
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以1-氨基-2-苯氧基-4-羟基蒽醌、氯磺酸、氯化亚砜、3-乙氧基丙胺为原料及Na2CO3为缚酸剂合成了C.I.分散红92。研究了氯磺酸、氯化亚砜用量及温度对氯磺化的影响,研究了3-乙氧基丙胺用量、pH值及温度对胺化缩合的影响。通过实验得到了较佳的反应条件,原料摩尔比是1-氨基-2-苯氧基-4-羟基蒽醌:氯磺酸:氯化亚砜:3-乙氧基丙胺为1:8:0.6:1;氯磺化温度为30℃~35℃;胺化缩合pH值为7~8,温度为15℃~20℃。并通过HPLC、1H-NMR、IR和MS对目标产品进行了分析。以1-氨基-2-苯氧基-4-羟基蒽醌计,总收率大于91%,目标产品HPLC纯度大于99%,溶剂回收率为95%。 相似文献
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以β-萘酚为原料,经醚化和Vilsmeier反应,合成了乙氧萘青霉素钠的侧链合成中间体2-乙氧基-萘醛,总收率90.2%,并对第二步Vilsmeier反应的合成工艺进行了改进,提高了收率,降低了废液的总磷、总氮和总量,提高了反应的环境友好性。 相似文献
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研究了(R)-1,1’-联萘-2,2’-二甲酸的合成方法,设计了一条合适的合成路线并进行了优化。以(R)-联二萘酚为起始原料,依次经过羟基的三氟甲基磺酸化反应、甲基化反应、溴代反应、水解反应,最后氧化成(R)-1,1’-联萘-2,2’-二甲酸。在相关文献和专利的基础上,进行了创新,合成路线简单易行,具有应用价值。 相似文献
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Most of the individual methylolmelamines that occur in melamine–formaldehyde adduct mixtures have been separated by preparative high-performance liquid chromatography (h.p.l.c.) and recovered in amounts sufficient to allow their characterisation by high-field 1H- and 13C-n.m.r. Particular attention has been paid to the chemical shifts of the aromatic azine carbons of the melamine nuclei. These carbon shifts are shown broadly to be in agreement with some values previously published, but additional assignments have been made. It is shown that a satisfactory quantitative analysis of the methylolmelamines in a melamine–formaldehyde adduct mixture can be carried out either by h.p.l.c. or by 13C-n.m.r. 相似文献
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High temperature, high pressure e.s.r. measurements of the hydrogenation reaction of Taiheiyo coal in the presence of catalysts were carried out to understand the stabilization of thermally and/or catalytically induced free radicals. A decrease in free radical concentration with increasing temperature was observed for ZnCl2 and SnCl2 · 2H2O catalysts at 10MPa under hydrogen gas. High pressure modified single-cell d.t.a. and p.d.a. equipment augmented the uniquely designed high temperature, high pressure e.s.r. cell. The hydrogenation reaction was monitored under the same experimental conditions as for e.s.r. From the results of the combination of high temperature, high pressure e.s.r. with high pressure d.t.a. and p.d.a., it was established that H2 molecules can react efficiently with free radicals from coal molecules created by the presence of ZnCl2 and SnCl2 · 2H2O catalysts. 相似文献
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The cycloaliphatic epoxy resins were studied by various two-dimensional nuclear magnetic resonance (2D n.m.r.) spectroscopies. The 13C n.m.r. spectra of the epoxy resins were assigned by using DEPT and 2D INADEQUATE techniques and the 1H n.m.r. spectra were assigned by using 2D 1H---1H and 1H---13C COSY techniques. Complete characterization of the samples synthesized by the oxidation of cyclohexene derivatives not only revealed the existence of the stereochemical isomers resulting from the structural difference of the oxide rings in the samples but also provided the composition ratio of the isomers. 相似文献
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An in-situ radical-quenching experiment was performed in an e.s.r. microwave cavity by using a solution flow system. Diphenylmethyl radicals produced from pyrolysis of 1,1,2,2-tetraphenylethane were quenched by several H-donor solvents. Among the solvents used, indan was the fastest in quenching, followed by hydrophenanthrene, tetralin, mesitylene and cumene in decreasing order of quenching rate. 相似文献
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The 1H and 13C nuclear magnetic resonance (n.m.r.) spectra of a delayed coking feedstock and products, presented in a previous paper, are analysed here in detail by matching results from inspection of both nuclei. The conventional spectra of whole samples are used in combination with elemental analysis data, and substantial agreement is obtained. Differences are explored to yield valuable information. Interpretation of some band assignments is modified to account for new results. This approach results in a detailed quantitative estimation of a few key structures that contain the main functional groups that characterize these petroleum fractions. 相似文献
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E.s.r. spectra of several oil shales from eastern and western USA have been measured at 9 and 25 GHz. The spectra of the western shales were similar to previously reported spectra and consist of a Mn2+ signal and a featureless organic signal. The eastern spectra consist of a V4+ signal and a complex and unusual organic signal consisting of at least four component signals. The organic signal has been characterized in terms of g factor, line-width and saturation characteristics. The effect of oxygen on the signal has also been examined. Electron nuclear double resonance (ENDOR) signals have been obtained from the organic signals of the eastern oil shales. 相似文献
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Akabira coal-derived neutral oil was separated into 25 narrow boiling range fractions covering 183–423 °C, and subsequently separated into compound class fractions : alkanes, monoaromatics, naphthalene-type diaromatics, fluorene-type diaromatics and tri- and/or tetraaromatics, by high performance liquid chromatography (h.p.l.c.). The compound type analyses of the distillate/h.p.l.c. fractions were performed using electron impact mass spectroscopy (e.i.m.s.) or field ionization mass spectroscopy (f.i.m.s.). Aromatic/hydroaromatic compound types and the alkyl side-chain carbon distribution of the distillate/h.p.l.c. fractions were clarified, based on the separation behaviour of h.p.l.c. and the type analyses according to Z value by m.s. By the distillation/h.p.l.c./m.s. method, coal-derived oil was characterized in terms of the distribution of the numbers of aromatic rings, naphthenic rings and carbons of alkyl groups attached to these rings. The variations in chemical structure in a compound class with distillation temperature are discussed in terms of these chemical structural factors. 相似文献
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Saudi Arabian heavy crude oil was separated into six fractions, including five distillate fractions (<93, 93–204, 204–260, 260–343 and 343–454 °C) and a >454 °C distillation residue. Each fraction was analysed by 1H and 13C n.m.r. spectroscopy, and combined gained information from these analyses provided reliable average structural parameters. These included estimation of aliphatic and aromatic content, average paraffinic chain length, and estimation of hydrogen, methyl and alkyl bearing aromatic carbons for each of the six fractions. The extent of branching in paraffinic chains and amount of aromatic bridgehead carbons were also calculated. 相似文献