Solvent effects in a carbenoid N-H insertion route to triarylamines via 2-diazo-1,3-cyclohexanedione

The Rh-carbenoid derived from 2-diazo-1,3-cyclohexanedione inserts into the N-H bond of arylalkylamines and diarylamines. A solvent for this reactive carbenoid is suggested. The insertion products undergo a Pd-mediated aromatization to afford alkyldiarylamines and triarylamines.     

Carboxamides of Dihydropyridin-2(1<Emphasis Type="Italic">H</Emphasis>)-ones

Summary. 3-Carboxamides and 3-carboxanilides of 6-alkyl and 6-aryldihydropyridin-2(1H)-ones have been prepared via different reaction pathways. All synthesized amides show hydrogen bonds in their NMR spectra. The 4-hydroxy compounds were obtained as a mixture of tautomers. Their configurations were elucidated by NMR experiments.Received December 16, 2002; accepted December 20, 2002 Published online June 2, 2003     

高密度发光材料BiTaO4∶Pr3+和BiTaO4的发光特性研究

研究了BiTaO4∶Pr3+, BiTaO4的光致发光性质, 测量了BiTaO4的红外透射和漫反射光谱. BiTaO4的光致发光光谱发射峰位于约420, 440, 465 nm; 其激发谱在约330～370 nm范围有明显的激发. BiTaO4∶Pr3+的光致发光光谱为Pr3+的特征发射, 主峰为606 nm, 来自Pr3+的3P0→3H6跃迁; 其激发谱由来自于基质的峰值为325 nm和范围在375～430 nm的宽激发带以及Pr3+的特征激发组成, 325 nm, 375～430 nm的激发带可能分别来自钽酸根团的电荷迁移跃迁和基质的带间缺陷能级的吸收; 在BiTaO4∶Pr3+中存在着基质→Pr3+的能量传递. 由于BiTaO4∶Pr3+基质的密度和Pr3+的发光强度均超过PbWO4, 因此BiTaO4∶Pr3+可能是潜在的重闪烁体.     

研磨法合成1,2,3,6-四氢嘧啶-2-酮衍生物

以NH₂SO₃H为催化剂, 室温无溶剂条件下, 研磨芳醛、β-酮酸酯和尿素合成了一系列1,2,3,6-四氢嘧啶-2-酮衍生物. 该方法具有反应条件温和、操作简便、环境友好、产率高等优点.     

液相色谱电化学安培检测乳粉中的脂溶性维生素A, E和D3

利用维生素A、D3、E均有电化学活性的特点,采用电化学安培检测,建立了HPLC检测奶粉中的脂溶性维生素A、D3、E的新方法.流动相为甲醇∶水=95∶5(V/V),含0.05 mol/L高氯酸钠.检测器采用玻碳电极,直流安培模式(DC),氧化电位 1.3 V.方法检测限为:VA、VD3、-αVE、-γVE、-δVE分别为0.08、2.3、0.16、0.19、0.28ng.回收率分别为:90.2%~98.2%、91.2%~103%、92.7%~99.5%、92.6%~97.4%、90.7%~98.0%.同紫外检测比较,方法具有灵敏度高、抗干扰强的特点.     

微波辐射下无催化剂一锅法合成N-甲基十氢吖啶-1,8-二酮化合物

为了研究从简单易得的原料在无催化剂的条件下一锅法合成N-甲基十氢吖啶-1,8-二酮化合物，我们以各类醛（脂肪醛、芳香醛、二醛）、达咪酮或1,3-环己二酮和甲胺为原料，以乙二醇或水为溶剂，经微波辐射，一步反应得到了一系列N-甲基十氢吖啶-1,8-二酮化合物。反应时间从传统热反应的4-5小时缩短至2-10分钟，产率较高（56-95%），并且不需要使用催化剂。该反应后处理方便，只需要简单洗涤，环境友好，为合成此类化合物提供了一种简便、有效的合成方法。该方法不仅适用于一元脂肪醛、芳香醛，还适用于芳香二醛，因此可以合成含有一个或两个十氢吖啶结构单元的杂环化合物。     

MZr2（AsO4）3（M=Na,K,Rb,Cs）的水热合成与结构表征

用水热晶化法合成了MZr_2(ASO_4)_3(M=Na,K,Rb,Cs)系列化合物。研究了反应物浓度、配比及不同砷源等水热晶化条件对产物物相的影响。用XRD、IR和Raman光谱对产物进行了表征。4种晶体的振动光谱由钠到铯呈现出规律性变化。     

Synthese und Geruch von Tricyclo[6.2.2.02, 7]dodecan-Derivaten

Summary The acetale-ketone9 was synthesized as precursor for the preparation of -santalol derivatives posessing a bicyclo[2.2.2]octane nucleus. After methylenation of the keto-group the subsequent acidic hydrolysis of the acetal leads via a Prins reaction of the liberated aldehyde with the methylene group to tricyclo[6.2.2.0^{2, 7}]dodecane derivatives. Their olfactory properties are described.

     

Spectrophotometric determination of Fe(II) in milligram solid samples

The analytical procedure of determination of Fe(II) in the presence of Fe(III) in milligram samples is proposed. A solid sample is dissolved in hydrochloric acid in argon atmosphere. Subsequently, the pH-value of the solution is fixed and Fe(III) complexed by phosphoric buffer. At the next step Fe(II) is oxidized by -molybdosilicic acid. Finally, the intensity of colouring caused by the reduced form of the acid is measured at the wavelength 770 nm. The proper treatment of the sample during oxidation, and immediately before, is decisive for the accuracy of the analysis. The method was verified by means of the analysis of synthetic magnetite. The theoretical content of Fe(II) was 24.12%, the determined one was 24.02 ± 0.10%. The method was applied to the determination of the homogeneity of an iron catalyst for ammonia synthesis.     

1－N－（苯并咪唑－1－乙酰基）－4－苯基－3－氨基硫脲金属配合物的合成及结构表征

合成了新配体１－Ｎ－（苯并咪唑－１－乙酰基）－４－苯基－３－氨基硫脲（ＢＰＭＳ），将其与Ｍｎ（Ⅱ）、Ｃｏ（Ⅱ）、Ｎｉ（Ⅱ）、Ｃｕ（Ⅱ）、Ｃｄ（Ⅱ）、Ｚｎ（Ⅱ）、ＵＯ２（Ⅱ）等金属的醋酸盐反应，合成了７个新配合物。所有化合物均经元素分析、ＩＲ、１ＨＮＭＲ和热重分析等表征。红外光谱表明，配体以四齿方式通过烯醇式羰基氧原子、烯醇式硫羰基硫原子以及Ｃ＝Ｎ１和Ｃ＝Ｎ２的氮原子与金属配位