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1.
以对硝基苯肼为起始原料,采用费舍尔吲哚合成法合成中间体5-硝基吲哚-2-羧酸酯(3),经还原合成5-氨基吲哚-2-羧酸酯(4),再与4-甲氧基-2-甲苯基异氰酸酯合成脲(5),(5)在水合肼作用下5-(3-(4-甲氧基-2-甲苯基)脲基)-1H-吲哚-2-碳酰肼(6),化合物6和取代醛反应,合成了6个2,5-二取代吲哚衍生物(7a~7f),其结构经~1HNMR,~(13)CNMR和HR-MS表征。采用MTT法研究了7a~7f对人肺癌细胞(A549)和人肝癌细胞(HepG-2)的体外抗增殖活性。结果显示:7d体外抑制活性最优,其IC_(50)分别为10.35μmol·L~(-1)、12.60μmol·L~(-1)。 相似文献
2.
《化学研究》2021,32(2)
以2-甲氧基-4-氟苯胺(2)为原料,用硝酸铵代替硝酸钾进行硝化反应得2-氟-4-甲氧基-5-硝基苯胺(3),进而与丙烯酰氯进行酰胺化反应得N-(2-氟-4-甲氧基-5-硝基)苯基-2-丙烯酰胺(4)。4与N, N, N-三甲基乙二胺进行亲核取代反应时,加入阻聚剂对羟基苯甲醚,成功地降低了副反应Michael加成反应的发生,得到N-[2-[[2-(二甲基氨基)乙基]甲基氨基]-4-甲氧基-5-硝基]苯基-2-丙烯酰胺(5)。用锌粉、无水氯化钙代替Pd/C催化对5的还原反应,产物不经纯化直接与3-(2-氯嘧啶-4-基)-1-甲基吲哚进行偶联得目标产品奥希替尼,总收率43.2%(以2计),纯度为99.85%。改进后的工艺路线步骤少、反应条件温和、操作和后处理简便,为奥希替尼的制备提供了一种新的方法。 相似文献
3.
4-(5-喹啉-3-基-四氮唑-2-基)丁胺的合成 总被引:1,自引:0,他引:1
三苯基膦钯催化3-溴喹啉完成氰化取代制得3-氰喹啉(1);1与叠氮化钠经[2+3]环加成合成了3-(2H-四氮唑-5-基)喹啉(2);2与N-(4-溴丁基)邻苯二甲酰亚胺反应制得2-[4-(5-喹啉-3-基-四氮唑-2-基)丁基]异吲哚-1,3-二酮(3);3经肼解合成了4-(5-喹啉-3-基-四氮唑-2-基)丁胺(4... 相似文献
4.
以N-甲基-4-硝基苯胺作为起始原料,依次经氯乙酰化、取代及氢化还原反应制得关键中间体N-(4-氨基苯基)-甲基-2-(4-甲基-1-哌嗪基)乙酰胺(4);以4-氯-3-硝基苯甲酸为原料,依次经酯化、取代、氢化还原及环合反应制得6-甲氧羰基-2-吲哚酮(8); 8与原苯甲酸三乙酯和乙酸酐经“一锅煮”反应制得中间体1-乙酰基-3-甲氧基(苯基)亚甲烯基-2-氧代吲哚环-6-羧酸甲酯(9); 4和9进行取代反应的同时脱除保护,经“一锅煮”反应合成尼达尼布,总收率57.2%,其结构经1H NMR,13C NMR和MS(ESI)确证。 相似文献
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5-,6-,7-硝基取代的3-吲(口乃木)乙酸已分别由Cavallini[1],Brown[2],Hiremath[3]与他们的合作者合成。本文报告从4-硝基吲(口乃木)通过相应的3-二甲氨代甲基吲(口乃木)(芦竹碱),按标准步骤合成4-硝基-3-吲(口乃木)乙酸。Berti等[4]曾用3-二甲氨代甲基吲(口乃木)直接硝化的方法制得4-硝基-3-二甲氨代甲基吲(口乃木)(4-硝基芦竹碱),熔点120—122°,产率很低。 相似文献
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以(S)-3-(2,2-二甲基-5-(3-甲基-1H-吲哚-2-基)-1,3-二氧杂环己烷-5-基)吡咯烷-2-酮为原料,经吡咯烷酮还原开环、串联的氢化脱保护/分子内还原胺化反应等关键步骤,合成了吲哚生物碱actinophyllic acid的A/B/C环手性中间体(S)-3-(2-(2-氯乙酰氨基)-2′,2′-二甲基-1,2,3,4,5,7-六氢螺[氮杂环辛烷并[4,3-b]吲哚-6,5′-[1,3]二氧杂环己烷]-5-基)-3-丙酮酸甲酯(9); 9可在氧化条件下转化为A/B/G环中间体(S)-7-(2-(2-氯乙酰氨基)乙基)-2′,2′-二甲基-8-氧代-7,8-二氢-5-H-螺[环庚烯并[b]吲哚-6,5′-[1,3]二氧杂环己烷]-9-甲酸酯(10)。该合成路线涉及9个新化合物,其结构经1H NMR,13C NMR, 2D NMR和LC-MS(ESI)表征。 相似文献
10.
合成了5-[N-(叔丁氧甲酰基)氨基]-1,3,3-三甲基-6′-硝基吲哚啉螺吡喃(BOCSPI)和5-[N-(叔丁氧甲酰基)氨基]-1,3,3-三甲基-6′-硝基-8′-甲氧基吲哚啉螺吡喃(BOCSPII)两种光致变色化合物,采用紫外-可见光谱法研究了其在溶液和以不同质量比掺杂在聚甲基丙烯酸甲酯(PMMA)膜中的光致变色性能.研究表明螺吡喃的高掺杂量不利于其开环和闭环态的转化,BOCSPII分子中的甲氧基有利于有色开环体的部花菁的稳定. 相似文献
11.
The sorption of artificial dye effluent made from two different dyes, Solar orange 7 GLL and Solar Jade Green FFB from Clariant,
onto three different agricultural residues—barley husk, sugarcane bagasse, and wheat straw—was studied. Twenty percent of
600-μm particle size of these agricultural residues was used as substrates and studied individually. The percentage of dye
removal was observed in concentrations of dye varying from 50 to 200 mg/L. The effect of temperature ranging from 25 to 50°C
and pH from 6.0 to 12.0 on the dye removal by the substrates was also studied. The effective adsorption of the substrates
was calculated. 相似文献
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Yoshiharu Aizawa Tsutomu Takata Minoru Kurihara Mamoru Tominaga Yoko Inoue 《应用有机金属化学》1988,2(4):395-398
In the manufacture of integrated circuits involving semiconductors, various hazardous materials including arsenic compounds are used. This paper present an evaluation of the biological monitoring of arsenic in the urine, blood and hair of semiconductor workers. Eighty-two blood samples were obtained from research and development workers in a semiconductor factory. Thirty-one samples of urine were obtained from the same group of worker before and after a work period (one shift). Seventy-three hair samples were similarly obtained from the workers. The concentration of arsenic in each sample was determined by arsine (AsH3) generation flame atomic absorption spectrometry after wet ashing of the sample. The mean concentration of arsenic in hair in these semiconductor workers was significantly higher than that of controls. The mean concentration of arsenic in hair from workers with a longer employment duration was higher than from those with a shorter employment duration. The mean concentration of arsenic in hair from workers engaged in epitaxial growth processes was higher than from workers engaged in other processes. The concentrations of arsenic in hair from semiconductor workers correlated with the duration of their employment. The mean concentration of arsenic in urine before a work a period (shift) was not significantly different from that of controls. The mean concentration of arsenic in urine after a work period was in fact lower than that of controls. The mean concentration of arsenic in blood was not significantly different from that of controls. The determination of arsenic in hair is therefore considered useful for the evaluation of relatively long-term exposure to arsenic in semiconductor workers. 相似文献
14.
H. Watson P. G. Mikkola J. B. Rosenholm J. G. Matisons 《Colloid and polymer science》2001,279(10):1020-1028
Industrial grade γ-ureidopropyltrimethoxysilane was adsorbed onto industrial grade E-glass fibres from toluene and carbon
tetrachloride at 23 °C. The treated surfaces were characterised using thermogravimetry, diffuse reflectance Fourier transform
IR spectroscopy, electron spectroscopy for chemical analysis, scanning electron microscopy and the zeta potential. When ureidosilane
was deposited from toluene and CCl4, both of which have very low hydrogen-bonding ability, a ureido surface was obtained. The ureidosilane deposited from CCl4 hydrolysed at the surface and condensed to form a solvent-swollen Si–O–Si network. The ureidosilane deposited from toluene
also hydrolysed at the E-glass surface. Condensation of the silane deposited from toluene was not apparent. Aluminium dissolved
from the E-glass surface was condensed into the network of the silane deposited from CCl4. Aluminium was not detected at the surface of the samples with ureidosilane deposited from toluene.
Received: 10 November 2000 Accepted: 23 March 2001 相似文献
15.
顶空固相微萃取-气相色谱-质谱联用分析纺织品中挥发性有机物 总被引:10,自引:0,他引:10
建立了顶空固相微萃取(HSSPME)-气相色谱(GC)-质谱(MS)联用测定纺织品中甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯5种挥发性有机物(VOCs)的分析方法。选择聚二甲基硅氧烷(PDMS)作为萃取涂层,优化了SPME的萃取条件,包括平衡时间、萃取时间、萃取温度、顶空体积、离子强度、搅拌速度、解吸温度和时间以及GC—MS仪器条件。对于甲苯、4-乙烯基环己烯、苯乙烯、萘和1-苯基环己烯方法线性范围分别为0.087~870、3.32~3320、2.28~2280、0.015~150和0.050~50.0ng/g;检出限分别为0.005、0.042、0.670、0.008和0.011ng/g。实际样品加标回收率在80.1%~122%之间,RSD在0.8%~8.6%之间。方法符合纺织品中痕量VOCs的快速分析要求。 相似文献
16.
鱼腥草中黄酮类成分的高效液相色谱指纹图谱分析 总被引:5,自引:0,他引:5
采用均匀实验设计和信息理论评价方法,建立了鱼腥草中黄酮类成分的高效液相色谱(HPLC)指纹图谱的分析方法。采用建立的方法和本研究室提出的指纹图谱评价软件,对同样种植条件下10个批次的鱼腥草指纹图谱进行了相似性评价,相似度均大于0.90;同时测定了芦丁、槲皮甙和槲皮素3个成分在10批鱼腥草药材中的含量分别为0.25%~0.34%、0.27%~0.37%、0.012%~0.016%。另外对不同采收季节和不同部位的鱼腥草药材中的黄酮类成分进行了指纹图谱的测定、主成分分析以及成分含量测定,结果表明,不同季节、不同部位的鱼腥草中黄酮类化合物的指纹图谱及成分含量存在较大的差异,且药用部位的差异大于采收季节的差异。该方法为规范鱼腥草中黄酮类成分在制药和用药的实际应用提供了一些可靠的基础信息。 相似文献
17.
免疫亲和色谱特异性剔除中药方剂四逆散中的柚皮苷 总被引:7,自引:0,他引:7
为了获得剔除柚皮苷(naringin)的中药方剂四逆散样品以供其药理活性探讨时使用,制备了抗柚皮苷抗体的免疫亲和色谱柱,用于特异性地剔除四逆散中的柚皮苷。首先合成了柚皮苷的完全抗原柚皮苷与牛血清白蛋白的结合物naringin-BSA,并用naringin-BSA对新西兰兔进行免疫获得抗血清,再将其纯化后与经CNBr活化的Sepharose 4B凝胶共价偶联制成免疫亲和色谱柱。将四逆散提取物样品溶液上样该色谱柱,洗脱,制得特异性剔除了柚皮苷的四逆散样品。由检测结果可知,naringin-BSA被成功合成。将其用于免疫新西兰兔,获得的抗血清的效价经酶联免疫吸附法(ELISA)测定达到1∶30000,抗体IgG的纯度达94%,交叉反应率低。在IgG与Sepharose 4B合成的IgG-Sepharose免疫亲和色谱柱中,IgG的偶联率为87%。用该免疫亲和色谱柱处理四逆散后,其中所含的柚皮苷几乎完全被剔除。结果证明,利用抗柚皮苷免疫亲和色谱,能特异性地剔除四逆散或其他样品中的柚皮苷成分。 相似文献
18.
The present work describes a novel method for the incorporation of Nile blue A into polyurethane foam matrix. This foam material was found to be very suitable for the extraction of metal ions from aqueous solutions. The characterization of Nile blue A grafted foam and the effect of halide concentration, pH, shaking time, extraction isotherm and capacity have been investigated. This foam material was found to be suitable for the separation and preconcentration of iron (III), zinc (II), cadmium (II) and mercury (II) from waste water. The extraction was accomplished in (15-20) minutes. Iron was separated from acid medium (2-4 M HCl), zinc from (3-5 M HCl), cadmium from (4-6 M HCl) as thiocyanate complexes and mercury was separated from (1-2 M HCl) as chloride. 相似文献
19.
The adsorption capacity for methanol-benzene andn-propanol-water mixtures was measured on two kinds of microcrystalline celluloses and cotton linters. Excess adsorption isotherms were obtained; the free energy of displacement was calculated from the isotherms. The enthalpy of displacement for one crystalline cellulose was measured by flow calorimetry. The entropic function of displacement was derived from the enthalpy and free energy of displacement. The preferential adsorption of methanol andn-propanol was characterized by the adsorption equilibrium constant.On leave from the Department of Physical and Colloid Chemistry, Wageningen Agricultural University, The Netherlands 相似文献