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以间二甲苯为原料,经氯甲基化、酯化、再水解成功制得新物质2,4,6-三(羟甲基)间二甲苯。利用FTIR、1H NMR、13C NMR等手段对产物的结构进行了表征。以间二甲苯计,三步反应的总收率达57.6%。 相似文献
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以易得的原料α-乙酰基-γ-丁内酯出发,通过甲基化、开环脱羧氯化、脱氯化氢关环、格氏反应、开环重排得到目标产物三甲基高烯丙基溴(TM);虽然反应步骤较多,但每步的收率都较高,操作简便,三甲基高烯丙基溴的总收率达到52.6%,为该化合物的合成提供了一条较好的合成路线,同时为谷氨酸毒性抑制剂苯扎思特事-E(Benzastatin-E)的全合成提供了重要的原料.此外对产物及中间体都进行了波谱解析与表征,确定了它们的结构. 相似文献
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以D-果糖为初始原料,经环合、氧化,再加入盐酸羟胺作为氰基化试剂一步法制得4(5)-氰基咪唑.利用1H NMR、13C NMR等手段对各步所得产物的结构进行了表征,结果表明产物为4(5)-氰基咪唑.以D-果糖计,3步反应的总收率为33.5%. 相似文献
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2-三氟甲基吡啶的合成与光谱表征 总被引:1,自引:0,他引:1
以2-氯基吡啶为原料,合成2-溴吡啶(收率68%)和2-碘吡啶(收率56%);2-溴吡啶和2-碘吡啶与三氟乙酸钾反应,得2-三氟甲基吡啶(收率56%-72%).通过NMR和元素分析对产物的结构进行了表征.该合成路线的优点是原料易得,反应条件温和,收率较高,总收率为38%-42%. 相似文献
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描述了一种有效的环境友好的“一锅煮”法合成13-乙酰基-9-甲基-11-羰基-8-氧代-10,12-二氮杂三环[7.3.1.0~(2,7)]十三碳-2,4,6-三烯。该法用廉价易得的溴化镁作催化剂,在无溶剂存在下,由起始原料水杨酸,乙酰丙酮和脲通过Biginelli缩合反应伴随着分子内的Michael加成反应一步完成。用核磁共振氢谱、碳谱、飞行时间质谱以及红外光谱数据表征了产物的结构为一氧桥多环化合物,而不是带有自由羟基的二氢嘧啶酮。最后由质谱给出的精确质量及其所代表的元素组成推出了该化合物的质谱裂解途径。 相似文献
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以苯并[1,2-b∶4,5-b´]二噻吩-4,8-二酮为原料合成了一种聚合物太阳能电池材料的单体2,6-双(三甲基锡)-4,8-双(2-乙基己氧基)苯并[1,2-b∶4,5-b´]二噻吩. 通过多核1D和2D NMR技术(包括1D 1H、13C、119Sn、117Sn NMR、DEPT、选择性1D TOCSY及2D1H-1H COSY、gHSQC、gHMBC)表征了目标分子结构,完成了 1H、13C、119Sn 与117Sn NMR化学位移归属,并探讨了该化合物的NMR谱线特征. 相似文献
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M Ramesh B Raju M George K Srinivas V Jayathirtha Rao K Bhanuprakash R Srinivas 《Journal of mass spectrometry : JMS》2012,47(7):860-868
The electrospray ionization collisionally activated dissociation (CAD) mass spectra of protonated 2,4,6-tris(benzylamino)-1,3,5-triazine (1) and 2,4,6-tris(benzyloxy)-1,3,5-triazine (6) show abundant product ion of m/z 181 (C(14) H(13)(+)). The likely structure for C(14) H(13)(+) is α-[2-methylphenyl]benzyl cation, indicating that one of the benzyl groups must migrate to another prior to dissociation of the protonated molecule. The collision energy is high for the 'N' analog (1) but low for the 'O' analog (6) indicating that the fragmentation processes of 1 requires high energy. The other major fragmentations are [M?+?H-toluene](+) and [M?+?H-benzene](+) for compounds 1 and 6, respectively. The protonated 2,4,6-tris(4-methylbenzylamino)-1,3,5-triazine (4) exhibits competitive eliminations of p-xylene and 3,6-dimethylenecyclohexa-1,4-diene. Moreover, protonated 2,4,6-tris(1-phenylethylamino)-1,3,5-triazine (5) dissociates via three successive losses of styrene. Density functional theory (DFT) calculations indicate that an ion/neutral complex (INC) between benzyl cation and the rest of the molecule is unstable, but the protonated molecules of 1 and 6 rearrange to an intermediate by the migration of a benzyl group to the ring 'N'. Subsequent shift of a second benzyl group generates an INC for the protonated molecule of 1 and its product ions can be explained from this intermediate. The shift of a second benzyl group to the ring carbon of the first benzyl group followed by an H-shift from ring carbon to 'O' generates the key intermediate for the formation of the ion of m/z 181 from the protonated molecule of 6. The proposed mechanisms are supported by high resolution mass spectrometry data, deuterium-labeling and CAD experiments combined with DFT calculations. 相似文献
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V. V. Nedel’ko B. L. Korsunskii T. S. Larikova S. V. Chapyshev N. V. Chukanov Shu Yuantsze 《Russian Journal of Physical Chemistry B, Focus on Physics》2016,10(4):570-575
The thermal decomposition of 2,4,6-triazido-1,3,5-triazine in the melt and a dinonyl phthalate solution is studied by thermogravimetry, manometry, mass spectrometry, and IR spectroscopy. The kinetic and activation parameters of the process are determined. The only gaseous product of the reaction is nitrogen. This fact, along with the structure of the condensed residue formed during the thermal decomposition of 2,4,6-triazido-1,3,5-triazine in the melt, are indicative of the abstraction of a nitrogen molecule from an azide group at the initial stage and of the subsequent reactions leading to the formation of a planar network of polyconjugated bonds between C and N atoms. For the thermal decomposition of 2,4,6-triazido-1,3,5-triazine in solution the preexponential factor and activation energy are found to be 1012.8 s–1 and 34100 cal/mol, respectively, which are characteristic of the thermal decomposition of most azides. To explain why these parameters are substantially higher for the reaction in the melt (1017.4 s–1 and 42300 cal/mol), it is assumed that, in this case, the process proceeds by the polymerization (polycondensation) mechanism to form twodimensional networks, with the apparent kinetic parameters being effective quantities. Based on these data, it is concluded that the high sensitivity of 2,4,6-triazido-1,3,5-triazine to external influences is of kinetic nature. 相似文献
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莪术醇进行环外双键断裂氧化和酸催化氧桥开环加成2步反应后,经硅胶柱层析分离,得到一种新型的莪术醇衍生物(2). 应用1D NMR和2D NMR测试了化合物2的1H NMR、13C NMR、1H-1H COSY、gHSQC、gHMBC,对化合物2的1H和13C化学位移进行了全归属,结合其红外光谱和质谱,推得化合物2为8-羟基-12-异丙基-2-甲基-三环[6.2.2.01,5]十二烷-10-氧杂-6,9-二酮,并比较了莪术醇,莪术醇双键断裂氧化产物(化合物1),化合物2的1H NMR、13C NMR数据变化. 相似文献
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A series of new high light fastness, hot pressing fastness optical brighteners was efficiently synthesized by a three-step approach involving the successive replacement of the three chloro groups of 2,4,6-trichloro-1,3,5-triazine under different conditions of temperature and pH. Thus, 2,4,6-trichloro-1,3,5-triazine was treated with different anilines and the resulting dichlorotriazinyl intermediates (3a-I) were further condensed with 4,4-diaminostilbene-2,2′-disulfonic acid to afford bis-monochlorotriazine (5a-I) followed by nucleophilic substitution with ethanolamine to furnish the final hybrid brighteners (7a-I). All of the newly synthesized compounds were characterized by Fourier-Transform Infrared (FT-IR), UV-visible absorption, NMR spectroscopy and the elemental analyses. The synthesized optical brighteners were also assessed for their efficacy as fluorescent brightening agents. 相似文献
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Radicals have been generated from the benzyl phenolic antioxidant 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl) benzene, carrying out oxidative and hydrogen abstraction reactions. Transient phenoxyl radicals were
directly visualized but only persistent carbon-centered radicals were monitored by electron paramagnetic resonance (EPR).
The experimental EPR results let us rationalize our analysis as the sum of two different radicals. One, called the methylene
radical, developed from the loss of a benzylic hydrogen gave place to a doublet of triplets witha
CHH≅2.7 mT anda
PHH=0.165 mT. Besides, the methyl radical, developed after an intramolecular hydrogen transfer involving a methyl group on the
central aromatic ring of the molecule, formed a triplet of triplets, witha
1H around 0.060 mT anda
2H=0.169 mT. All the contact interactions were tested by EPR simulation of the experimental data. 相似文献
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M. D. Threadgill 《Isotopes in environmental and health studies》2013,49(3):143-144
Treatment of N,N,N′,N′,N″-Pentamethyl-1,3,5-triazin-2,4,6-triamin with butyllithium and trideuteroiodomethane give N,N,N′,N′,N″-Pentamethyl-N″-(trideuteromethyl)-1,3,5-triazin-2,4,6-triamin, a deuterated analogue of the anticancer drug hexamethylmelamine, in high yield. 相似文献
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采用密度泛函理论的M062X方法和6-311G(d,p)基组,对苯乙烯与苯酚的反应进行了分子轨道理论计算。通过讨论反应过程中各分子的最高占据轨道(HOMO)和最低空轨道(LUMO),预测了化学反应的方向和相应的反应产物。经过前线轨道理论分析,得出苯乙烯与苯酚反应的关键步骤是形成苯乙烯基碳正离子,反应中H+起到催化作用;反应产物主要有4-(1-苯基乙基)苯酚、2-(1-苯基乙基)苯酚、2,4-双-(1-苯基乙基)苯酚分子、2,4,6-三-(1-苯基乙基)苯酚(SP-3)、1,3-二苯基丁烯和4-(1,2-二苯丙基)苯酚。 相似文献
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采用密度泛函理论的M062X方法和6-311G(d,p)基组,对苯乙烯与苯酚的反应进行了分子轨道理论计算.通过讨论反应过程中各分子的最高占据轨道(HOMO)和最低空轨道(LUMO),预测了化学反应的方向和相应的反应产物.经过前线轨道理论分析,得出苯乙烯与苯酚反应的关键步骤是形成苯乙烯基碳正离子,反应中H+起到催化作用;反应产物主要有4-(1-苯基乙基)苯酚、2-(1-苯基乙基)苯酚、2,4-双-(1-苯基乙基)苯酚、2,4,6-三-(1-苯基乙基)苯酚(SP-3)、1,3-二苯基丁烯和4-(1,2-二苯丙基)苯酚. 相似文献
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Journal of Fluorescence - In the current study, on the basis of 1,3,5-tris(2-methylimidazol-1-yl)benzene (timb), a designed tripodal connector, two new transition metal coordination polymers (CPs),... 相似文献
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Gumann S Nestle N Liebau-Kunzmann V Riedel R 《Solid state nuclear magnetic resonance》2007,31(2):82-90
Lithium-containing silicon (oxy)carbonitride ceramics (SiCN(O):Li) were synthesized via precursor-to-ceramic-transformation of Li-containing (poly)silazanes. The precursors were obtained by lithiation of 2,4,6-trimethyl-2,4,6-trivinylcyclotrisilazane with n-butyllithium and by reaction of a commercial poly(organosilazane) VL20 with metallic lithium. The annealing treatment was carried out at temperatures between 200 and 1400 degrees C in argon (DeltaT=200 degrees C) and yielded Li-containing silicon (oxy)carbonitride. X-ray powder diffraction revealed that the resulting SiCN(O):Li ceramics were basically amorphous up to temperatures of 1000 degrees C and formed LiSi(2)N(3), graphite and silicon carbide as crystalline phases at higher temperatures. (7)Li MAS NMR spectroscopy was carried out to investigate the structure of the Li-containing phases and to study the reaction path of metallic Li with polysilazane. Based on the NMR spectra, there is almost no difference found in the chemical shift of the SiCN(O):Li ceramics obtained at different temperatures. Accordingly, Li is assigned to be mainly coordinated to N and O present as contaminant element. Relaxation time measurements showed that the most mobile Li(+) species seems to be present in the product obtained in the pyrolysis temperature range between 600 and 1000 degrees C. 相似文献