共查询到19条相似文献,搜索用时 125 毫秒
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以3,4-二甲氧基苯甲醛为原料,在二氯亚砜作用下,一步反应合成得到目标产物2-氯-3,4-二甲氧基苯甲醛,其结构经1 HNMR和GC-MS确证。对影响目标产物收率的因素进行了考察,确定的最佳反应条件为:物料n(3,4-二甲氧基苯甲醛)∶n(二氯亚砜)=1∶1.3,反应溶剂为二氯甲烷,反应温度为-30℃,反应时间为16h。在此最佳反应条件下,目标产物的收率为63.4%。 相似文献
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研究了以3-氯-5-甲氧基-2,6-二硝基吡啶为原料,通过甲氧化、硝化、氨化合成3-甲氧基-5,6-二氨基-2-硝基吡啶,该化合物的结构通过IR,1H NMR,MS和元素分析进行了表征,确认为目标化合物。分析了3-甲氧基-5-氯-2,6-二硝基吡啶的氯基和硝基的反应活性。 相似文献
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以3,4-二甲氧基苯甲醛为原料,经过Darzens缩合、碱解、脱羧3步反应合成了3,4-二甲氧基苯乙醛,总收率为58.3%。并与甲醇和乙二醇分别缩合,合成了4-(2,2-二甲氧基乙基)-1,2-二甲氧基苯和2-(3,4-二甲氧基苄基)-1,3-二氧戊环两种羰基保护物。 相似文献
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2,5-二甲氧基苯乙胺合成方法的改进 总被引:2,自引:0,他引:2
以锌粉和氯化高汞作还原剂、2,5-二甲氧基苯甲醛为原料,与硝基甲烷在少量吡啶存在下,合成了2,5-二甲氧基-β-硝基苯乙烯,将其还原得到目标产物2,5-二甲氧基苯乙胺。通过对不同还原剂对反应影响的讨论可知,采用锌粉和氯化高汞作还原剂总收率可提高到62·5%。 相似文献
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Summary The 2,3-dimethylene-1,3-butadiene dianion (2) was prepared from 2,3-dimethyl-1,3-butadiene (1) using Lochmann's base (n-BuLi/potassium-t-butoxide in pentane). The dianion was reacted with primary halides to yield 2,3-disubstituted-1,3-butadiene monomers. These monomers were polymerized free radically with AIBN and with Ziegler/Natta coordination catalysts. The resulting polymers were examined by DSC for crystallization of the polymer backbone and alkyl side chains. 相似文献
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首次从2,3-二甲氧基-1,3-丁二烯衍生物出发,微波辐射下采用一锅法成功合成了一系列3,4-乙撑二氧噻吩类化合物.实验表明,该法具有反应条件温和、收率高和操作简单的优点.3,4-乙撑二氧噻吩类化合物的结构经 ~1HNMR 、~13CNMR、IR和元素分析进行了表征.也讨论了原料的量、催化剂和溶剂对3,4-乙撑二氧噻吩(EDOT)收率的影响. 相似文献
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溴化苄和叠氮化钠为原料,通过叠氮化反应制得叠氮苄,反应收率达73.6%。2,3-二溴-1,1,1-三氟丙烷为原料,通过烯化、炔基化制得1-苯基-4,4,4-三氟-2-丁炔-1-醇,反应收率达75.5%。1-苯基-4,4,4-三氟-2-丁炔-1-醇和叠氮苄,在[Cp*RuCl2]n催化下通过1,3-偶极环加成反应首次合成了标题化合物,反应收率达到89.2%。产物结构经IR、1HNMR、19FNMR、13CNMR、ESI-MS和元素分析确证。 相似文献
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Summary Reaction of E-1,4-poly(2-triethylsilyl-1,3-butadiene) (I) with m-chloroperbenzoic acid (MCPBA) yields E-1,4-poly(2,3-epoxy-2-triethylsilyl-1,3-butadiene) (II). Similar reaction of E-1,4-poly[2,3-bis(trimethylsilyl)-1,3-butadiene] (III) with MCPBA gives E-1,4-poly[2,3-epoxy-2,3-bis(trimethylsilyl)-1,3-butadiene] (IV). The product polymers have been characterized by 1H, 13C, and 29Si NMR, IR, GPC, TGA and elemental analysis. 13C and 29Si NMR permit Stereochemical analysis on the microstructures of II and IV. 相似文献
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A series of bifunctional ZnCe@SBA-15 catalysts with different Zn/Ce ratios were prepared by a solid-state grinding strategy and used in the conversion of ethanol to 1,3-butadiene (ETB). For the supported metal oxides, ZnO serves as the active sites for the dehydrogenation of ethanol, and CeO2 promotes the aldol-condensation reaction. Based on the results of Py-FTIR and NH3-TPD, it suggests that the yield of 1,3-butadiene is positively correlated with the number of weak Lewis acid sites on the catalyst surface, given their benefit for aldol-condensation reactions. The catalyst with an optimal Zn/Ce ratio of about 1:5 has the highest concentration of weak Lewis acid. Coupling with the ZnO sites, it contributes to a 98.4% conversion of ethanol and a 45.2% selective of 1,3-butadiene under relatively mild reaction conditions (375 ℃, 101.325 kPa, and 0.54 h-1). 相似文献
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Xu Hou Bochong Chen Zhenzhou Ma Jintao Zhang Yuanhang Ning Donghe Zhang Liu Zhao Enxian Yuan Tingting Cui 《中国化学工程学报》2022,42(2):389-398
Due to the complexity of feedstock, it is challenging to build a general model for light olefins production. This work was intended to simulate the formation of ethylene, propene and 1,3-butadiene in alkanes pyrolysis by referring the effects of normal/cyclo-structures. First, the pyrolysis of n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane, cyclohexane, methylcyclohexane, n-hexane and cyclohexane mixtures, and n-heptane and methylcyclohexane mixtures were carried out at 650-800℃, and a particular attention was paid to the measurement of ethylene, propene and 1,3-butadiene. Then, pseudo-first order kinetics was taken to characterize the pyrolysis process, and the effects of feedstock composition were studied. It was found that chain length and cyclo-alkane content can be qualitatively and quantitively represented by carbon atom number and pseudo-cyclohexane content, which made a significant difference on light olefins formation. Furthermore, the inverse proportional/quadratic function, linear function and exponential function were proposed to simulate the effects of chain length, cycloalkane content and reaction temperature on light olefins formation, respectively. Although the obtained empirical model well reproduced feedstock conversion, ethylene yield and propene yield in normal/cyclo-alkanes pyrolysis, it exhibited limitations in simulating 1,3-butadiene formation. Finally, the accuracy and flexibility of the present model was validated by predicting light olefins formation in the pyrolysis of multiple hydrocarbon mixtures. The prediction data well agreed with the experiment data for feedstock conversion, ethylene yield and propene yield, and overall characterized the changing trend of 1,3-butadiene yield along with reaction temperature, indicating that the present model could basically reflect light olefins production in the pyrolysis process even for complex feedstock. 相似文献
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用小型密闭压力容器实验(MCPVT)分别跟踪测定了1,3-丁二烯在氮气和氧气氛围下温度随时间的变化(T-t)和压力随时间的变化(p-t)。利用p-t曲线构建了1,3-丁二烯初期氧化反应动力学。结果表明,在氮气条件下,即使温度达到388.15 K也未检测到1,3-丁二烯发生化学反应。1,3-丁二烯与氧气在343.15~363.15 K范围内发生了氧化反应,反应器内的压力减小。1,3-丁二烯与氧气的初期氧化反应动力学是二级反应。另外,还考察了氧气过量和1,3-丁二烯过量时两种特殊情况下的假一级氧化反应动力学。探讨了过渡态的热力学参数,计算结果表明,1,3-丁二烯的热氧化是一个有序的分子数减少过程。用气相色谱-质谱联用仪和碘量法分析了氧化反应产物,其产物有呋喃和过氧化物。 相似文献