美金刚胺衍生物的合成

以盐酸美金刚胺为原料,分别与对硝基苯甲酰氯,苄氧羰基缬氨酸经酰基化反应和催化加氢反应,合成了两个新型的美金刚胺衍生物——N-对氨基苯甲酰基美金刚胺和缬氨酰基美金刚胺,其结构经1H NMR和IR表征。     

邻甲酰胺基苯甲酰胺类化合物的合成

以邻硝基苯甲酸或对氯邻硝基苯甲酸为原料,经酰氯化、胺化、还原、胺解4步反应,合成了6个新的邻甲酰胺基苯甲酰胺类化合物,总收率66%～73%,其结构经1 H NMR, MS和元素分析表征.     

新型N-(2'-芳胺嘧啶-4'-基)-N,2,3-三甲基-2H-吲唑-6-胺衍生物的合成及其抗肿瘤活性

以3-甲基-6-硝基-1H-吲唑为原料,经N-甲基化、催化还原、亲核取代及烷基化反应制得关键中间体N-(2'-氯嘧啶-4'-基)-N,2,3-三甲基-2H-吲唑-6-胺(5);5与芳胺经亲核取代反应合成了一系列新型的N-(2'-芳胺嘧啶-4'-基)-N,2,3-三甲基-2H-吲唑-6-胺衍生物,其结构经1H NMR和MS确证。初步生物活性测试结果表明,部分化合物具有明显的抗肿瘤活性。     

新型溴乙酰四胺化合物的合成

以四胺盐酸盐和2-溴乙酰溴为起始原料,在碳酸钾和二氯甲烷/水中通过缩合反应合成了两个新型溴乙酰四胺化合物,其结构经1H NMR和MS表征.     

六亚甲基四胺法合成芳甲基胺

以卤甲基芳烃和六亚甲基四胺为原料。合成了芳甲基胺。收率90％以上。其结构经^1H NMR表征。     

含可聚合基团的萘酰亚胺衍生物的合成

以4-溴-1,8-萘酐和4-硝基-1,78-萘酐为起始原料,与各种芳胺经亚胺化,再与脂肪胺经取代反应,最后与丙烯酰氯经酯化得到一系列具有强烈荧光的含丙烯酰氧乙基氨基的1,8-萘酰亚胺衍生物,它们可作为一种聚合荧光色素的单体。     

空穴传输材料三芳胺衍生物的合成及性质研究

以二芳胺和芳碘体系为原料,经乌尔曼反应制备了一系列三芳胺衍生物,经NMR,IR,MS等表征了其结构,通过示差扫描量热法(DSC)测定了其玻璃化转变温度,并利用循环伏安法结合紫外可见光谱测定了其HOMO能级和LUMO能级.     

(5-甲基-2-烷氧基苯基)-1-烃基胺的合成

以对甲酚(1)为起始原料,经醚化、酰化和还原氨化反应合成了5个(5-甲基-2-乙氧基苯基)-1-烃基胺;1经酯化、Fries重排、醚化和还原氨化反应合成了5个(5-甲基-2-甲氧基苯基)-1-烃基胺.其结构经1H NMR,13C NMR,IR和GC-MS表征.     

沙利多胺与叶酸偶联物的合成研究

本文报道了沙利多胺与叶酸偶联物的合成方法。以廉价易得的邻苯二甲酸酐和谷氨酰胺为原料通过酰化、环合反应得到沙利多胺,沙利多胺与37%甲醛溶液通过羟甲基化反应得到N-羟甲基沙利多胺,再与N-羟基琥珀酰亚胺(NHS)活化的叶酸通过偶联反应得到目标化合物。合成的关键中间体和目标化合物的物性与文献一致,其结构经核磁共振氢谱确认。     

三烯胺催化2,5-二烯酮的远端不对称Mannich反应

利用三烯胺机制活化环状2,5-二烯酮,对远端的不对称Mannich反应进行研究。用手性伯胺催化环状2,5-二烯酮原位生成三烯胺中间体,与苯甲醛和苯胺经三组分一锅法反应获得了7个新型的远端不对称Mannich加成产物,其结构经¹H NMR, ¹³C NMR和HR-MS(ESI)表征。在最佳反应条件下,收率达87%,对映选择性达78%。     

Preparation and properties of polyurethane networks based on α,ω-difunctional poly(hexafluoropropylene oxide)

Poly(hexafluoropropylene oxide), poly(HFPO), networks were prepared from functional polymers by end linking via urethane groups. The prepolymers were characterized by NMR spectroscopy and GPC. The networks were characterized by determination of the number of network chains from the shear modulus, and were snown to contain both trifunctional crosslinks and difunctional links. The properties of the networks were investigated by a range of techniques. Compared with fully-fluorinated networks formed via triazine cross-links, investigated previously, the urethane-linked networks were more readily prepared but were poorer elastomers, were less thermally stable, and were less resistant to swelling by common polar solvents. © 1995 John Wiley & Sons, Inc.     

南瓜籽烘烤前后化学成分的分析

对烘烤前后南瓜籽中的化学成分进行分析并对比。采用同时蒸馏萃取装置萃取南瓜籽中的挥发性成分,采取超临界CO2萃取技术萃取南瓜籽油脂,并将其分为酸、碱、中性三个部分,用气相色谱-质谱联用方法分析其中化学成分并进行对比。结果表明,南瓜籽挥发性成分中含有多种醛类和酯类化合物,烘烤后产生了大量的烷基吡嗪,其在碱性部分中的相对含量比烘烤前提高14倍多,不饱和醛类化合物含量也有明显提高。南瓜籽油脂中的主要化学成分是油酸、亚油酸及其酯类。还含有生物活性功能成分如植物甾醇、角鲨烯和维生素E等。烘烤后除角鲨烯含量有所降低,维生素E、植物甾醇、亚麻酸等均有提高。     

云南菊科中草药中铅含量特征分析

论述了云南２７种菊科中草药及其水提取物中铅含量的特征。菊科植物及水提物中铅含量的频数分布为正偏态,两者的相关系数ｒ＝０．０９,未呈现显著的线性相关。提取率较高的山紫苑、佩兰、木香铅实际含量低;铅含量高的叶下花、狭叶兔耳风、臭灵丹提取率又较低,减少了人体对Ｐｂ的过量摄入。     

幼儿身高、体重和头发、血液锌铅含量关系的研究

同步检测了151例3-4岁健康幼儿的身高、体重以及头和全血中的锌、铅含量。研究了身高、体重和锌、铅含量的关系,指出无论是发锌或血锌含量与身高、体重多数呈正相关,但发铅与身高、体重主要呈负相关,血铅与身高、体重的关系较为复杂,多为非线性的二次函数关系。     

碳苷研究 V: 用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护

本文报道了一些取代苯酚的合成, 并探讨了用Grignard试剂合成取代苯酚中酚羟基的保护及脱保护的问题. 利用苄基和甲基作为酚羟基的保护基, 对文献报道的切断醚键脱保护方法进行了评价. 找到了两种新体系能在更温和条件下切断醚键的方法, 指出了它们的适用条件. 实验结果符合硬软酸碱理论.     

膜催化研究II. 多孔无要膜的制备与表征及其反应器对甲醇脱氢反应的促进作用

采用溶胶-凝胶法制备了多孔氧化铝膜, 并通过DSC、TGA、SEM、N~2吸附和气体透过率测定等手段, 对膜的性能进行了表征。结果表明, 用这种方法制备的多孔氧化铝膜是一种均匀无裂痕和具有较窄孔径分布(约4nm)的膜材料。将此多孔氧化铝膜制成膜反应器后, 用于甲醇催化脱氢制甲醛的反应, 发现甲醇转化率比常规反应器有较大幅度的提高。同时首次尝试采用溶胶-凝胶法将催化活性组分直接负载到多孔氧化铝膜上, 从而得到了一种具有催化活性的多孔膜, 并考察了它的反应活性。文中对由这两种多孔膜及钯/陶瓷复合膜制成的反应器的特点进行了比较。     

Determination of Geosmin and 2-Methylisoborneol in Water by Headspace Liquid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

Geosmin (GSM) and 2-methylisoborneol (MIB) were extracted from water samples, adsorbed in organic solvent microdrop by headspace liquid-phase microextraction (HS-LPME), and were analyzed by gas chromatography-mass spectrometry (GC-MS). Influence factors such as the extraction solvent types, headspace and microdrop volumes, stirring rate, equilibrium and extraction time, and ionic strength for HS-LPME efficiency were thoroughly evaluated. Under optimized extraction and detection conditions, the calibration curves of GSM and MIB were linear in the range of 5–1000 ng/L. The detection limits of GSM and MIB were 1.1 and 1.0 ng/L, respectively. Average recoveries of 95.45–113.7% (n = 5) were obtained and method precisions were also satisfactory. Trace levels of the off-flavor compounds at ng/L in tap water and raw water were successfully quantified.     

FT-IR, FT-Raman spectra, density functional computations of the vibrational spectra and molecular geometry of biomolecule 5-aminouracil

FT-IR and FT-Raman spectra of the biomolecule 5-aminouracil were recorded in the regions 400–4000 cm⁻¹ and 10–3500 cm⁻¹, respectively. The observed vibrational wavenumbers were analyzed and assigned to different normal modes of vibration of the molecule. Density functional calculations were performed to support wavenumber assignments of the observed bands. A comparison with the molecule of uracil was made, and specific scale factors were employed in the predicted wavenumbers of 5-aminouracil. With the purpose of study the important molecule 5-aminouracil, its equilibrium geometry and harmonic wavenumbers were calculated for the first time by the B3LYP DFT method. The vibrational wavenumbers were compared with IR and Raman experimental data. Also good reproduction of the experimental wavenumbers is obtained and the % error is very small. All the tautomeric forms of 5-aminouracil were determined and optimized. The dimer forms were also simulated. The energy, atomic charges and dipole moments were discussed and several general conclusions were underlined.     

玩具、铅笔中可溶性砷、锑、硒的形态分析

对玩具、铅笔中可溶性砷、锑、硒的形态分析方法进行了研究,对原子荧光光谱法测定不同价态砷、锑、硒的方法进行了优化,建立了砷、锑、硒的原子荧光光谱形态分析方法。该方法样品加标回收率为82.0%~110.0%,测定结果的相对标准偏差为1.35%~2.22%(n=10)。     

Group contributions to the infinite dilution partial molar volumes of alkanes, alcohols, and glycols in polar organic solvents

Densities of binary mixtures of polar organic solvents with alcohols were measured at 25‡C. The solvents studied were N,N-dimethylformamide, dimethylsulfoxide, and formamide while alcohols were butanol, pentanol, hexanol, and 1,4-butanediol. Density measurements of hydrocarbons (from pentane to dodecane and some heptane isomers) + N,N-dimethylformamide were also performed. From these data the apparent molar volumes of alcohols and hydrocarbons as functions of concentration were calculated. The standard partial molar volumes were obtained by extrapolation to infinite dilution and are discussed in terms of group contributions.