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在对糖苷的FAB分析技术的研究中发现,如果在样品中同时加入适量的NaCl和LiCl水溶液进样时,其 FAB 谱中会出现[M+Na]~+和[M+Li]~+两个强峰,两峰之质量差为16(Na 和 Li 原子量之差值),并且发现其谱图中找不到明显的碎片离子和 Na~+及 Li~+的加合离子,而只有糖苷分子和Na~+及 Li~+的加合离子.所以很容易在 FAB 谱中识别它们,因而不需联谱解析而仅凭 FAB 谱就可准确、快速地定出糖苷的分子量.此技术国内外尚未见报道. 相似文献
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在对糖苷的FAB分析技术的研究中发现,如果在样品中同时加入适量的NaCl和LiCl水溶液进样时,其FAB谱中会出现[M+Na]^+和[M+Li]^+两个强峰,两峰之质量差为16(Na和Li原子量之差值),并且发现其谱图中找不到明显的碎片离子和Na^+及Li^+的加合离子,而只有糖苷分子和Na^+及Li^+的加合离子。所以很容易在FAB谱中识别它们。因而不需联谱解析而仅凭FAB谱就可准确、快速地定出糖苷的分子量。此技术国内外尚未见报道。 相似文献
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本文研究了八种含1—3个糖基的糖苷的负离子快原子轰击(NFAB)质谱.NFAB质谱与相应的正离子谱(PFAB)比较,在高质量区示出较明显的准分子离子[M-H]~-峰而无加合离子峰,从而能较明确指示糖苷的分子量.在所试验的三种底物甘油、硫代甘油和聚乙二醇-200(PEG-200)中,以PEG-200给出的结果最佳.[M-H]~-离子的碰撞活化谱(NFAB-CA谱)产生的特征离子比[M+H]~+离子PFAB-CA谱中相应离子的丰度大,能更为明确地给出糖基连接顺序信息. 相似文献
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研究了八种含1一3个糖基的糖苷的负离子快原子轰击(NFAB)质谱,NFAB质谱与相应的正离子谱(PFAB)比较,在高质量区示出较明显的准分子离子[M-H][-]峰而无加合离子峰,从而能较明确指示糖苷的分子量, 在所试验的三种底物甘油、硫代甘油和聚乙二醇-200(PEG-200)中,以PEG-200给出的结果最佳,[M-H][-]离子的碰撞活化谱(NFAB-CA谱)产生的特征离子比[M+H][+]离子PFAB-CA谱中相应离子的丰度大,能更为明确地给出糖基连接顺序信息。 相似文献
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本文报道了二个低价钼簇合物的快原子轰击(FAB)和电子轰击(EI)质谱:(Et_4N)_2[Mo_2(CO)_8(μ-SPh)_2]的FAB和FAB—NI谱及Mo_2(CO)_8(μ-SPh)_2的FAB和EI谱。分别获得它们的完整的配位阳离子和阴离子峰。这类簇合物的大致裂断解途径可能是首先脱CO、然后脱C_6H_5—,在EI—MS谱中观察到双金属离子裂解为单金属碎片离子的反应。文中探讨了质谱条件下标题簇合物的氧化还原反应。研究结果同时表明,Mo价态明显影响碎片离子峰的相对丰度和Mo对配位体CO、—SPh、—S的络合能力。另外,还报道了Mo_2(CO)_6(μ-SPh)_2(CH_3CN)_2的FAB—MS和EIMS谱。 相似文献
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寡糖快原子轰击质谱中碱金属加合离子应用技术的研究 总被引:1,自引:0,他引:1
生命科学的研究成果[1~3]表明,糖蛋白和糖脂中的糖基可作为细胞的识别信号,能控制细胞的分裂和分化.快原子轰击(FAB)质谱是测定寡糖的重要手段[4,5],但目前还存在不少问题.我们在对麦芽各糖的研究中. 相似文献
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本文研究游离胆汁酸及其丁二酸衍生物的快速原子轰击(FAB)质谱.用甘油或硫甘醇作样品的基质,具有不同的灵敏度增强效应。FAB负离子质谱,获得[M-n]-典型离子簇,[M-1]-作为最强离子是每一个样品的基峰. 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