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提出以三氟乙酸酐作为衍生化试剂,将核黄素半合成中间体N-(D)-脱氧核糖醇基-3,4-二甲苯胺(Ⅰ)及4,5-二甲基-N-(D)-脱氧核糖醇基-2-偶氮苯基苯胺(Ⅱ)转化为低沸点易汽化物质,采用以苯乙酮作为内标,测定中间体(Ⅰ)和(Ⅱ)纯度的气相色谱法。方法具有分析速度快、准确度高、重现性好等优点,方法回收率(Ⅰ)为96.9% ̄101.2%、(Ⅱ)为99.4% ̄100.4%,相对标准偏差(Ⅰ)在4 相似文献
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以固体酸为催化剂,4,4’-二氟二苯甲酮与苯胺脱水缩合,合成了N-(双(4-氟苯基)亚甲基)苯胺.比较了不同固体酸催化剂H型ZSM-5、Na型ZSM-5、介孔分子筛MCM-41(Al)及强酸型离子交换树脂Amberlyst 15的催化效果.使用比表面、NH3-TPD对催化剂进行了表征,并与催化效果关联.考察了催化剂用量、原料摩尔比、浓度及溶剂等反应条件对产物收率的影响.产物通过熔点、核磁共振谱进行了表征.结果表明,HZSM-5固体酸催化剂具有优异的催化作用.在优化条件下,以对二甲苯为反应溶剂和脱水剂,4,4’-二氟二苯甲酮0.1 mol,苯胺0.2 mol,催化剂用量2.0 g,反应24 h,产物收率达91%.此外,催化剂易于分离,能够重复使用多次. 相似文献
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合成了2-(4-甲基苯基)-3-(N-乙酰基)-5-(2-羟基苯基)-1,3,4-噁唑啉(MPAHO),并用核磁共振波谱法和红外光谱法对其进行了表征。采用荧光光谱技术研究了MPAHO与人血清白蛋白(HSA)的相互作用。结果表明:MPAHO对HSA有较强的荧光猝灭作用,根据Stern-Volmer方程得到的荧光猝灭常数,可判断由于与MPAHO反应而导致HSA的荧光猝灭均属于静态猝灭。采用位点结合模型公式和Frster非辐射能量转移理论计算了结合常数、结合位点数、结合距离。从计算得到的热力学参数焓变ΔH和熵变ΔS,推断MPAHO与HSA之间的作用力为静电引力。并应用同步荧光光谱和三维荧光技术研究了MPAHO对HSA构象的影响。 相似文献
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5-烃基-2,3-二甲基吡嗪N-单氧化物的合成 总被引:1,自引:0,他引:1
一烃基或二烃基吡嗪的N-单氧化物可以进行氯化、乙酰氧基化等反应,它是重要的有机合成中间体.据报道二烃基吡嗪与30%过氧化氢在醋酸中进行N-氧化反应,当二烃基吡嗪:30%过氧化氢:醋酸的摩尔比为1:2:5、反应温度70~80℃、反应时间8h时,产物是N-单氧化物;当摩尔比为1:4:10、反应温度95℃、反应时间8~24h时,产物是N-二氧 相似文献
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应用自制的ECL-1型电致化学发光仪,对新试剂5-(对-苯胺偶氮)-2,3-二氢-1,4-酞嗪二酮(简称ADPD)在Na_2CO_3-NaHCO_3-H_3BO_3缓冲介质中的电化学发光行为作了研究。结果表明,当介质pH值为10.20时,在各种选定的实验条件下,施加+2.0V(vs.SCE)三角波脉冲电压,体系发光强度与ADPD浓度在2×10~(-9)~1×10~(-7)mol/L范围内呈线性关系。反应的检测限为5×10~(-10)mol/L。并且提出了ADPD电化学发光的可能机理。 相似文献
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以对称二氨基硫脲为原料,与冰醋酸反应生成5-甲基-4-氨基-1,2,4-三唑-3-硫酮(1);在弱酸性条件下,1与取代水杨醛反应生成席夫碱中间体5-甲基-4-(N-取代邻羟苯基)亚胺基-1,2,4-三唑-3-硫酮(2a~2c);最后在碱性条件下分别与N-取代苯基-2-氯乙酰胺发生烷基化反应生成15种未见报道的目标化合物3-(N-取代苯基-2-乙酰胺基)硫基-4-(N-取代邻羟苯基)亚胺基-5-甲基-1,2,4-三唑(3a~3o),其结构经IR,1H NMR,13C NMR确证.初步生物测试表明,质量分数为0.01%时,3a~3o对白色念珠菌的抑菌率均达90%以上,具有很强的抑菌活性;对金黄色葡萄球菌、大肠杆菌的抑菌率达80%以上,具有较强的抑菌活性. 相似文献
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以3,5-二溴吡啶和对甲基苯硼酸为原料,醋酸钯为催化剂,经Suzuki偶联反应合成了3,5-二(4-甲基苯基)吡啶(1),收率73%,其结构和性能经1H NMR, 13C NMR, IR, 元素分析, UV-Vis, FL和X-射线单晶衍射表征。结果表明:1(CCDC: 1509844)属正交晶系,空间群P212121,晶胞参数a=6.447 8(12) , b=7.240 2(14) , c=29.890 0(6) ,β=90°。1为非平面刚性共轭分子,荧光量子产率13.9%。 相似文献
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对(4R-cis)-6-[2-[2-(4-氟苯基)-5-(1-异丙基)-3-苯基-4-[苯胺(羰基)]-^1H-吡咯-1-基]乙基]-2,2-二甲基-1,3-二氧己环-4-乙酸叔丁酯的傅里叶变换离子回旋共振质谱(FT-ICR-MS)、核磁共振氢谱(^1H-NMR)、碳谱(^13C-NMR)以及^1H同核位移相关谱(^1H-^1HCOSY)、检出^1H的异核多量子相干谱(HMQC)和^1H检测的异核多键相关谱(HMBC)报道并进行解析。确定了^1H谱、^13C谱中各谱峰的归属,研究了其六元环部分的立体构象,并就空间效应对其化学位移的影响做了初步的探讨。 相似文献
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以乙酰基二茂铁为原料,经3步反应合成了一个新型的二茂铁衍生物——2,2-二甲基-1-[5-二茂铁基-3-(三氟甲基)-1H-吡唑-1-基]丙-1-酮(4),其结构经1H NMR,ESI-MS,元素分析和X-射线单晶衍射表征。4属单斜晶系,P2(1)/c空间群,晶胞参数a=7.805 6(4),b=20.906 1(11),c=11.124 6(6),β=93.820(2)°,V=1 811.33(17)3,Z=4,Dc=1.482 g·cm-3,μ=0.872 mm-1,R1=0.034 8,wR2=0.089 2。采用循环伏安法研究了4的电化学性质。结果表明:4有一对可逆的氧化还原峰,Epa=0.640 V,Epc=0.482 V,ΔE=153 m V。 相似文献
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The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound. 相似文献
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Irina O. Zhuravel Oleg V. Zaremba Oleksandr S. Detistov Svitlana S. Kovalenko Valentin P. Chernykh 《合成通讯》2013,43(21):3778-3784
New 5-hydroxymethyl-8-methyl-3-(3-aryl-[1,2,4]oxadiazol-5-yl)-2H-pyrano-[2,3-c]pyridin-2-ones and their esters were synthesized. The structure of obtained compounds was determined through a complete 1H NMR analysis. 相似文献
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The corresponding 1-(2-quinoxalyl)-, 1-[3,5-di(trifluoromethyl)phenyl]-, and 1-ethoxycarbonyl-3-methyl-4-oxo-4,5,6,7-tetrahydroindazoles have been obtained from reactions of 2-acetyl-1,3-cyclohexanedione, its 5,5-dimethyl and 5-(2-furyl) derivatives, with 2-hydrazinoquinoxaline, 3,5-di(trifluoromethyl)phenylhydrazine, and ethoxycarbonylhydrazine. On interaction with ethoxycarbonylhydrazine the intermediate 2-[1-(-ethoxycarbonyl)hydrazino]ethylidene-1,3-cyclohexanediones were also isolated. From the potassium salt of 2-formyldimedone and 2-carboxyphenylhydrazine hydrochloride, 2-(2-carboxyphenyl)hydrazinomethylene-5,5-dimethyl-1,3-cyclohexanedione was obtained, the cyclization of which in ethanol in the presence of HCl led to 1-(2-carboxyphenyl)- and 1-(2-ethoxycarbonylphenyl)-6,6-dimethyl-4-oxo-4,5,6,7-tetrahydroindazole. 相似文献
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《Analytical letters》2012,45(16):1343-1354
Abstract Electrochemical monitoring of 1, 4-dihydroxy-5, 8-bis-[2-(2-hydroxyethy1) aminoethy amino]-9, 10-anthracenedione was employed for the quantitation of this cancer chemotherapy drug following high performance liquid chromatography. Detection was performed by oxidation of the compound at a glassy carbon electrode at +0.80 V vs. SCE. A rapid and convenient sample treatment procedure was developed which is suitable for determination involving physiological samples. A detection limit of 2 ng injected was obtained for urine samples. 相似文献
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E. Karthikeyan S. Perumal s. Selvaraj 《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2379-2386
Diastereoselective synthesis of a series of (Z)-1-[3-aryl-2-(phenylsulfanyl)-2-oxiranyl]-1-ethanones was effected from the reaction of (Z)-4-aryl-3-(phenylsulfanyl)-3-buten-2-ones with alkaline hydrogen peroxide in tetrahydrofuran. The stereochemistry of the oxiranes has been deduced from two-dimensional NOESY spectrum. 相似文献
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Xin Bo ZHOU Cui Fang LIN Song LI 《中国化学快报》2005,16(10):1301-1304
The synthesis of (S)-2-(3-arylacrylamido)-3-{4-[2-(5-methyl-2-phenyloxazol-4-yl)etho- xy]phenyl}propanoic acids is described. Their structures were confirmed by ^1H-NMR. 相似文献