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101.
TheBeckInannrearrangement,theacid-mediatedisomerizationofoximestoamides,wasfirstdiscoveredinl886l.Asoneoftheoldestandmostfamiliartransformationsinorganicchemistry,ithasbeenwidelystudiedandagreatvarietyofmethodstoconductthistfansformationhavebeenreported'.However,mostofthesemethodswerecarriedoutbyusingalargeamountofsolventswithlongreactiontime.Whatismore,thepriorpreparationofthecorrespondingketoximesisusuallyrequired,whichmakestheseprocessesinconvenientandlessattractive.Bytakingadvantageofboth… 相似文献
102.
The interaction between gatifloxacin mesylate (GM) and salmon sperm DNA was studied by fluorescence spectrometry and ultra‐violet (UV) spectrometry. Additions of salmon sperm DNA to GM solution resulted in its strong fluorescence quenching and UV absorbance decrease due to the strong interaction between GM and salmon sperm DNA. Both the maximum fluorescence emission wavelength and the maximum UV absorbance wavelength of GM did not change with the increasing concentration of salmon sperm DNA, indicating no intercalative binding existed between them. The Stern‐Volmer plot indicated that the fluorescence‐quenching constant at different temperatures or different salmon sperm DNA concentration ranges was different. Effects of ionic strength and I? on the fluorescence quenching of GM by salmon sperm DNA indicated that electrostatic interaction and groove binding coexisted between them. 相似文献
103.
高稳定性CaO-ZrO2固体碱催化剂的表征和催化性能 总被引:3,自引:0,他引:3
用共沉淀法经高温焙烧制备了CaO摩尔分数从10%至50%的CaO-ZrO2系列催化剂, 将其应用于碳酸丙烯酯和甲醇酯交换合成碳酸二甲酯过程, 并通过XRD, FT-IR, BET, ICP, CO2-TPD, XPS等表征手段研究了催化剂的物性及其催化性能随组成变化的的规律. 结果表明, 当CaO摩尔分数高于30%时, 表面出现游离的CaO, 虽然具有强碱性和高活性, 但是稳定性差; 而当CaO摩尔分数低于30%时, Ca2+进入ZrO2晶格, CaO与ZrO2形成连续固溶体, 并且随着CaO含量的增加, 晶格氧的电荷密度增加, 催化剂的碱性增强, 使得CaO-ZrO2催化剂在碳酸丙烯酯和甲醇酯交换合成碳酸二甲酯过程中获得了高活性和高稳定性. 相似文献
104.
从唇形科植物铁轴草中分离得去甲克罗烷二萜化合物Teucvidin,通过催化氢化、酯交换、水解等反应合成了8个衍生物,用^1HNMR、MS和IR确定了其结构,初步生物活性测定结果表明,化合物Ⅱ和Ⅳa的拒食作用显著。 相似文献
105.
Sesquiterpene esters from the fruits of Celastrus orbiculatus 总被引:1,自引:0,他引:1
Three new beta-dihydroagarofuran sesquiterpene esters, 6 alpha-acetoxy-9 beta-benzoyloxy-1 beta-cinnamoyloxy-8 beta-butanoyloxy-beta-dihydroagarofuran (1), 6 alpha-acetoxy-9 beta-benzoyloxy-1 beta-cinnamoyloxy-8 beta-(2-methylbutanoyloxy)-beta-dihydroagarofuran (2), and 6 alpha-acetoxy-1 beta,8 beta-dibenzoyloxy-9 beta-hydroxy-beta-dihydroagarofuran (6), together with three known compounds (3-5) were isolated from the fruits of Celastrus orbiculatus THUNB. Their structures were elucidated on the basis of spectroscopic methods. Compound 4 showed moderate activity in inhibiting LPS-induced nitric oxide production in murine macrophage RAW264.7 cells with an IC(50) value of 43.7 microM. 相似文献
106.
Yunhui Zhai Xijun Chang Yuemei Cui Ning Lian Shoujun Lai Hong Zhen Qun He 《Mikrochimica acta》2006,154(3-4):253-259
A rapid, selective method that utilize 4-(2-Pyridylazo)-resorcinol (PAR)-modified nanometer SiO2 (nanometer SiO2–PAR) as a new solid-phase extractant for preconcentration of trace mercury (II) has been developed. The adsorption property
of nanometer SiO2–PAR for metal ions was studied by selectively extracting different metal ions from aqueous solutions. The results revealed
an excellent affinity of the nanometer SiO2–PAR for mercury (II) in presence of interfering metal ions at pH 4. The main parameters of solid-phase extraction such as
shaking time, elution and sample dilution effect were studied. The extractant shows rapid kinetic sorption, and the adsorption
equilibrium of mercury (II) on nanometer SiO2–PAR was achieved in less than 2 min. The adsorbed mercury (II) was easily eluted by 4 mL of 6 mol L−1 HCl. The maximum preconcentration factor was 50. The maximum static adsorption capacity was 276 μmol g−1 at pH 4. The detection limit (3σ) was 0.43 μg L−1 for cold vapor atomic absorption spectrometry (CVAAS), and the relative standard deviation of the eight replicate determinations
was 2.4% for the determination of 2.0 μg of Hg(II) in 100 mL water sample. The method was applied to the determination of
trace mercury (II) in sample solutions with satisfactory results. 相似文献
107.
本文报道了一种新的简便的合成N-乙基α-甲基-间苯乙胺的方法。方法以三氟甲苯为原料,经氯甲基化,Gignard及Leuckart反应后得目标物,具有原料价廉易得,毒性较小,反应条件温和,工艺流程较短等特点。 相似文献
108.
A direct synthesis of denbinobin 总被引:1,自引:0,他引:1
Denbinobin was made in seven steps from quinone 3. The cyclization of aldehyde 12 using P4-tBu and the oxidation of a hindered alcohol with MnO2 were key steps. 相似文献
109.
Deng C Li N Wang X Zhang X Zeng J 《Rapid communications in mass spectrometry : RCM》2005,19(5):647-653
In the current work, a simple, rapid, accurate and inexpensive method was developed for the determination of acetone in human blood. The proposed method is based on derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), followed by headspace liquid-phase microextraction (HS-LPME) and gas chromatography/mass spectrometry (GC/MS). In the present method, acetone in blood samples was derivatized with PFBHA and acetone oxime formed in several seconds. The formed oxime was enriched by HS-LPME using the organic solvent film (OSF) formed in a microsyringe barrel as extraction interface. Finally, the enriched oxime was analyzed by GC/MS in electron ionization (EI) mode. HS-LPME parameters including solvent, syringe plunger withdrawal rate, sampling volume, and extraction cycle were optimized and the method reproducibility, linearity, recovery and detection limit were studied. The proposed method was applied to determination of acetone in diabetes blood and normal blood. It has been shown that derivatization with HS-LPME and GC/MS is an alternative method for determination of the diabetes biomarker, acetone, in blood samples. 相似文献
110.