共查询到20条相似文献,搜索用时 62 毫秒
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研究了在水/有机物两相体系中水溶性钯-膦配合物催化柠檬酸的加氢反应。考察了反应温度、氢气压力、底物和催化剂浓度、反应时间、水相pH值等对该反应的影响,并与几种柠檬醛衍生物的加氢结果进行了比较。发现仅用蒸馏水作水相,则主要产物是二氢香茅醛(〉93%);而水相水加入Na2CO3后,则主要产物为香茅醛(97%),且加氢速度比同样条件下使用Pd/C催化剂快得多。 相似文献
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紫外分光光度法测定肉桂醛、苯甲醛和苯甲酸 总被引:4,自引:0,他引:4
根据肉桂醛、苯甲醛和苯甲酸的紫外吸收光谱特征及肉桂醛和苯甲醛在228 nm和256 nm波长处有两个等吸收点,提出了测定三组分的紫外分光光度法.选择228 nm,256 nm及311 nm 3个波长作为测定波长,建立了联立方程组,求得了组分浓度与吸光度之间的关系:C内桂醛=(A311 nm-0.008 4)/0.042 4;C笨甲醛=(A256 nm-0.000 5)/0.062 2-C内桂醛;C苯甲酸=(A228 nm+0.005 7)/0.061 1-C内桂醛-C苯甲醛.相应的线性范围依次在18.03,13.08,9.233 mg·L-1以内.对方法的重现性作了试验,上述3种化合物的相对标准偏差(n=6)均小于1%.用标准加入法进行回收试验,测得其平均回收率在99.1%~100.5%之间. 相似文献
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柠檬醛的非均相催化氢化:二氢香茅醛的制备 总被引:4,自引:0,他引:4
对含有多个可被还原的官能团化合物的催化氢化,难以找到既有高活性又具有高度选择性的催化剂。柠檬醛分子中含有两个碳碳双键和一个醛基,随氢化条件的不同可能生成下列4种产物: 相似文献
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阴离子交换树脂担载氟离子催化合成假性甲基紫罗兰酮 总被引:2,自引:0,他引:2
用阴离子交换树脂担载氟离子催化柠檬醛与丁酮的反应,合成了假性甲基紫罗兰。探讨了催化剂用量、反应物配比、反应温度和反应时间等因素对收率的影响,在柠檬醛为100mmol,n(柠檬醛):n(丁酮)=1:10,催化剂用量为柠檬醛质量的75%,室温反应1h的最佳反应条件下,产物收率87.1%,纯度99.1%。 相似文献
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建立了工业用苯乙烯中总醛含量测定的气相色谱分析方法。采用气相色谱-质谱全扫描模式对工业用苯乙烯样品进行定性分析,确定苯乙烯中存在苯甲醛、苯乙醛及苯乙酮等3种醛酮化合物,其含量顺序为苯甲醛苯乙醛苯乙酮。采用气相色谱-氢火焰离子化检测法对3种醛酮化合物检测,并用外标法定量。苯甲醛、苯乙醛及苯乙酮分别在5.8~221.5 mg/kg、0.7~26.1 mg/kg、0.6~24.1 mg/kg浓度范围内呈良好的线性(r20.9999);加标回收率为104.3%~111.8%,相对标准偏差为0.6%~2.0%(n=5);检出限为0.061~0.078 mg/kg,总醛的检出限(以苯甲醛计)为0.2 mg/kg。 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction. 相似文献
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The Diels-Alder reactivity of 1,2-heteroborines (H4C4B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed. 相似文献