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以2-乙氧基乙胺和3-氯-1-丙醇等为起始原料, 经7步反应, 制备了N,N-二[二(3-甲氧基丙基)膦基乙基]-2-乙氧基乙胺(PNP5)盐酸盐, 其中关键步骤是后两步. PNP5盐酸盐的结构和组成通过IR, 1H NMR, 13C NMR, 31P NMR, MS和元素分析等方法确认. 相似文献
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为研究高海拔种植大马士革玫瑰的化学成分,采用95%乙醇为溶剂进行连续回流提取,并采用硅胶、聚酰胺、C18及Sephadex LH-20凝胶等材料行分离纯化,最终得到了9个黄酮醇类化合物(1, 3, 5~11)和两个黄酮类化合物(2和4),其结构经1H NMR和13C NMR表征并结合理化方法鉴定为:5,7-二羟基-3,6,4'-二甲氧基黄酮醇(1)、 5,7-二羟基-6,4'-二甲氧基黄酮(2)、 5,7,4'-三羟基-3,6-甲氧基黄酮醇(3)、 5,7-二羟基-6,8,4'-三甲氧基黄酮(4)、 5,4'-二羟基-3,6,7-二甲氧基黄酮醇(5)、 5,7-二羟基-3,6,8,4'-三甲氧基黄酮醇(6)、 8-甲氧基山奈酚(7)、山奈酚(8)、槲皮素(9)、槲皮素 3-O-a-L-阿拉伯呋喃糖苷(10)、银锻苷(11),其中化合物1~5为首次从蔷薇属植物中分离得到,化合物1~7、 10、 11为首次从大马士革玫瑰中分离得到。
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报道了一种斑蝥素的常压合成方法。以3-氧代-4-甲酸甲酯四氢噻吩为起始原料,经氰基化和腈醇脱水反应制得3-氰基-4-甲酸甲酯-2,5-二氢噻吩(1); 1水解制得2,5-二氢噻吩-3,4-二羧酸(2); 2在二氯亚砜作用下脱水制得关键中间体2,5-二氢噻吩-3,4-二羧酸酐(3); 3依次经D-A反应和Raney Ni催化加氢的脱硫反应合成了斑蝥素(5),总收率38%,其结构经1H NMR, 13C NMR和MS(ESI)确证。研究了离子液体、反应时间和反应温度对D-A反应的影响。确定D-A反应的较优条件为:[BMIM]·BF4为离子液体,于35 ℃反应20 h,斑蝥素前体产率为86%。 相似文献
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Suleimenov E. M. Raldugin V. A. Shakirov M. M. Bagryanskaya I. Yu. Gatilov Yu. V. Kulyjiasov A. T. Adekenov S. M. 《Russian Chemical Bulletin》2003,52(5):1210-1212
Oxidation of (+)-sabinol, (1S,3R,5S)-1-isopropyl-4-methylidenebicyclo[3.1.0]hexan-3-ol, by active MnO2 afforded not the expected sabinone but only its [4+2]-cyclodimer. The molecular structure of the latter was established by X-ray diffraction analysis. The 1H and 13C NMR spectra of this cyclodimer were interpreted using 2D NMR spectroscopy. 相似文献
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Thomas Bräuniger C. Vinod Chandran Ulrich Wedig Prof. Dr. Martin Jansen 《无机化学与普通化学杂志》2011,637(5):530-535
Aluminium carbide, Al4C3, was characterised by 13C and 27Al solid‐state NMR spectroscopy. The 13C NMR spectra display two resonances with an intensity ratio of 1:2, which is in agreement with the reported crystal structure. The 27Al NMR spectra of Al4C3 under both static and MAS conditions were deconvoluted into two spectral components, belonging to the two aluminium species Al1 and Al2 in the crystal structure of Al4C3. The spectral fit allowed for determination of the relatively large quadrupolar coupling constants (χ ≈? 16 MHz) of both 27Al species. One aluminium species displayed a tendency of having a χ of slightly smaller magnitude compared to the other. By carrying out DFT calculations of the EFG tensor at the 27Al sites using the Wien2k software, we could tentatively assign the smaller χ site to be the crystallographic Al1 species. Also, the isotropic chemical shift for the carbon‐coordinated aluminium in Al4C3 could be determined, being in the range of 111 to 120 ppm. This is somewhat larger than those shift values observed for 27Al in nitrogen coordination. 相似文献
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Takehiko Yamato Carol Pérez-Casas Shofiur Rahman Zeng Xi Mark R. J. Elsegood Carl Redshaw 《Journal of inclusion phenomena and macrocyclic chemistry》2007,58(1-2):193-197
A novel receptor possessing two complexation sites and bearing 1,3-alternate conformation based on thiacalix[4]arene, confirmed by single crystal X-ray analysis, was prepared. The tetrathiacalix[4]arene
diamide shows strong intramolecular hydrogen bonding. The binding behavior towards K+ and halides has been examined by 1H NMR titration experiments. 相似文献
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Substituted 5-aryl-3-ethylidene-3H-pyrrol-2-ones were synthesized by the reaction of the corresponding 4-aryl-4-oxobutanoic acids with ketones in the presence
of aminating agents. The conditions of this reaction were developed with the use of both the conventional condensation technique
and microwave activation. The structures of the reaction products were con-firmed by elemental analysis, IR spectroscopy,
and 1H NMR spectroscopy.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 693–696, April, 2006. 相似文献
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N-[2(3)-Hydroxyalkylj-4-thiazolidinones have been synthesized by the reaction of 2(3)-vinyloxyalkylamines with mercaptoacetic acid in 24–69 % yield. The structure of the compounds obtained was supported by (R and1H NMR spectroscopic data.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 677–679, March, 1996. 相似文献
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V. F. Mironov T. A. Zyablikova I. V. Konovalova M. G. Khanipova R. A. Musin 《Russian Chemical Bulletin》1997,46(2):355-357
The products of reaction ofo-phenylenedioxytrichlorophosphorane with arylacetylenes were identified as 4-aryl-2-chloro-2-oxo-5,6-(4-chlorobenzo)phosphorin-3-enes
using1H,13C,31P NMR, and IR spectroscopy and high-resolution mass spectrometry.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 368–370, February, 1997. 相似文献
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J. Couquelet M. Madesclaire F. Leal V. P. Zaitsev S. Kh. Sharipova 《Chemistry of Heterocyclic Compounds》2001,37(7):898-902
The reaction of (1S,2S)-2-amino-1-(4-nitrophenyl)-1,3-propanediol with glutaraldehyde has been studied. It has been established on the basis of AM1 and PM3 calculations and 1H NMR spectra recorded in the presence of the shift reagent Eu(fod)3 that (1S,3S,4S,7R,11R)-3-(4-nitrophenyl)-11-aza-2,6-dioxatricyclo[5,3,1,04,11]undecane is formed as the result of the reaction. 相似文献
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5-HT3 receptor antagonists, such as Ondansetron, are used for anti-emesis after chemotherapy, radiotherapy and operations. Some
Ondansetron analogs possessing piperazine ring as side chains were synthesized in our lab. Thus, one of the two carbonyl groups
of starting material 1,3-cyclohexandione (1) was condensed with phenylhydrazine hydrochloride to form monophenylhydrazone (2). 1,2,3,9-Tetrahydro-4H-carbazol-4-one (3) was prepared from 2
via cyclization and rearranged in the presence of ZnCl2. Through a methylation reaction, compound 3 was converted to 1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one (4). 3-Dimethylaminomethyl substituted compound (5) was synthesized from 4 by a Mannich reaction in glacial acetic acid. Nine novel 1,2,3,9-tetrahydro-9-methyl-3-(4-substituted-piperazin-1-ylmethyl)-4H-carbazol-4-one derivatives (6a–6i) were synthesized through nucleophilic substitution reaction of 5 with piperazines. The structures of all the target compounds were determined by elemental analysis, IR, MS, 1H NMR and 13C NMR spectra. The results of preliminary pharmacological test show that part of the novel compounds have antiemetic activity
comparable to that of the control Ondansetron.
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Translated from Chinese Journal of Organic Chemistry, 2008, 28(2) (in Chinese) 相似文献
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为了寻找新的高活性农药, 利用工业易得的三氟羧草醚及其中间体为起始原料, 设计合成了9个未见报道的N-取代苯甲酰基-N'-取代芳基硫脲化合物, 结构经IR, 1H NMR, 元素分析确认. X射线衍射测定了化合物4b的晶体结构, 结果表明: 其分子属于三斜晶系, 空间群P-1, a=0.51588(19) nm, b=1.0766(4) nm, c=2.0596(8) nm, α=81.113(6)°, β=89.702(6)°, γ=78.131(6)°, V=1.1056(7) nm3, Dc=1.445 Mg/m3, Z=2, F(000)=492, μ=0.319 mm-1. 初步生物活性测试结果表明, 部分化合物具有较好的除草活性. 相似文献