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合成了2,6-二甲基-3,5-二乙氧羰基-1,4-二氢吡啶,并研究了它在紫外光(366nm)照射下的光化学反应。结果表明,主要的光化产物为2,6-二甲基-3,5-二乙氧羰基吡啶(占95%)其次是少量的二-π甲烷光重排产物,1,3-二甲基-2-氮杂-4,5-二乙氧羰基-双环-[3、1、0]-己烯-3(占5%)。 相似文献
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1,8-二羟基-9,10-二氢蒽的合成 总被引:1,自引:0,他引:1
以1,8-二羟基蒽醌为原料,经甲醚化,锌粉和金属钠还原,去甲基等4步反应合成1,8-二羟基-9,10-二氢蒽,总产率为37.1,8-二甲氧基蒽醌用NaBH4/CF3COOH还原生成二聚产物,并测定了其单晶结构. 相似文献
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1,1-二氨基-2,2-二硝基乙烯的合成研究进展 总被引:1,自引:0,他引:1
1,1-二氨基-2,2-二硝基乙烯(FOX-7)是一种低感度高能量的新型含能材料.现有的1,1-二氨基-2,2-二硝基乙烯的合成包括以2-甲基咪唑、盐酸乙脒与乙二酸二乙酯、2-甲基-4,6-二羟基嘧啶为前体的三条合成路线.使用硫酸/硝酸体系硝化2-甲基-4,6-二羟基嘧啶可得到2-二硝基亚甲基-5,5-二硝基嘧啶-4,6-二酮,然后水解可得到FOX-7,正相硅胶薄层色谱可对该反应进行监测.使用曲拉通X-100/正己烷体系的反相微乳法可制备FOX-7球形纳米晶;FOX-7球形纳米晶具有良好的应用前景,对其合成工艺与路线进行探索和研究具有一定的意义. 相似文献
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5,5-二甲基-2-氧代-2-(N,N-对苯二胺基-二苄基)-二-1,3,2-氧磷杂环己烷的合成及表征 总被引:1,自引:0,他引:1
以新戊二醇、三氯化磷和乙醇为原料制得中间体 5 ,5 -二甲基 -1 ,3,2 -二氧磷杂环己烷 -2 -氧 ( DPDO) ,用DPDO与由芳醛和对苯二胺缩合制得的席夫碱 SB ~ SB 加成 ,合成了膨胀型阻燃剂 5 ,5 -二甲基 -2 -氧代 -2 -( N,N -对苯二胺基 -二苄基 ) -二 -1 ,3,2 -氧磷杂环己烷 ( DPPO ~ DPPO ) ,通过元素分析 ,IR,NMR和 MS对其结构进行表征 ,并对其在醇酸清漆中的应用进行了讨论 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献