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采用锌-柠檬酸氢二铵溶液还原体系,以偶氮苯为原料合成出氢化偶氮苯.合成反应的最佳反应条件:当偶氮苯用量是0.625 mmol时,偶氮苯与锌的物质的量之比为1:5,0.2 g/mL柠檬酸氢二铵溶液用量5.0 mL,室温,时间约3 min,平均收率90.63%. 相似文献
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热能是最普遍的能量形式。典型的贮热材料是水合盐及其低共熔物,如Na2SO4·10H2O,CaCl2·6H2O等,它们在从固体向液体熔化时,可吸收大量的热。但此类材料有易发生相分离,过冷较严重,贮热性能易衰退的缺点[1]。当今固—固相变贮热成为研究的热点[2,3]。硫氰化铵从室温加热到150℃发生相变过程中,无液相生成,且具有较宽的固—固转变温度,较高的固—固转变焓,过冷度轻,无腐蚀,稳定性好,因而是一种理想的贮热材料[4]。硫氰化铵在加热过程中的相变行为是[5]:NH4SCN(单斜Ⅳ)ΔNH4SCN(正交Ⅲ)ΔNH4SCN(四方Ⅱ)ΔH2NS… 相似文献
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钒是具有重要用途的元素 ,其测定受到重视。二安替比林甲烷类[1]及杂环偶氮苯酚类显色剂[2 ,3]测定钒灵敏度和选择性较高 ,变色酸偶氮类显色剂[4 6 ]的应用也曾有报道 ,而杂环偶氮苯甲酸类显色剂研究较少[7,8]。本文研究了钒 (Ⅴ )与 2 (2 噻唑偶氮 ) 5 二甲氨基苯甲酸 (TAMB)的显色反应 ,结果表明 ,在 pH 3 .5 3 .8甲酸 NaOH缓冲介质中 ,钒(Ⅴ )与TAMB反应生成一种稳定的可溶于水的蓝色配合物。1 试验部分1.1 仪器与试剂72 1型分光光度计pHS 2型酸度计钒 (Ⅴ )标准溶液 :用偏钒酸铵 (NH4 VO3)水溶后配成含钒 1… 相似文献
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以聚丙烯腈纤维(PAN)为原料,氢化铝锂为还原剂,先将PAN上的腈基还原为伯胺基团得到还原产物PAN-NH2(APAN),再与具有季铵结构的2,3-环氧丙基三甲基氯化铵(EPTAC)键合,制备出季铵键合PAN聚合物;最后通过氢氧化钠活化得到具有强碱性季铵基团的聚合物PAN-N+(CH3)3OH-(QPAN).考察了氢化铝锂、EPTAC加入量及反应时间、温度等因素对季铵基键合量(—N+(CH3)2Cl-含量)的影响规律,采用X-射线光电子能谱(XPS)、红外光谱(FTIR)、示差扫描量热仪(DSC)等对聚合物结构和性能进行表征.结果表明,当PAN与还原剂氢化铝锂摩尔比为1∶3,温度为80℃,反应时间为24 h时,伯胺基团含量可达到0.4812mmol/g.进一步用还原产物APAN与EPTAC以最优反应条件(摩尔比1∶3,温度80℃,反应时间12 h)下进行反应,所得产物通过NaOH活化,得到碱强度为0.8034 mmol/g的QPAN.将QPAN用于大豆油和甲醇的酯交换反应制备生物柴油.在反应温度60℃,反应时间4 h,醇油摩尔比为16∶1,QPAN添加量为2.0 meq(OH-)的条件下,生物柴油产率可达64.7%. 相似文献
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用甲基三辛基氯化铵和钨酸钠一步法合成甲基三辛基季铵钨酸盐离子液体[(CH3)N(n-C8H17)3]2W2O11,以该离子液体为催化剂,在无反应溶剂条件下催化过氧化氢氧化苯甲醇生成苯甲酸。 考察了反应温度、催化剂用量以及氧化剂过氧化氢用量对苯甲酸产率的影响。 确定优化条件:反应温度70 ℃,苯甲醇用量5 mmol,催化剂用量是底物的0.4%(摩尔分数),30%过氧化氢用量2 mL,苯甲醇的转化率可达99%,苯甲酸选择性为98%。 该方法具有反应条件温和、产率高和选择性好的优点。 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