Synthesis and Crystal Structure of a Genistein-derived Compound

A genistein derivative, 5-hydroxy-3-（4-hydroxyphenyl）-7-（2-（piperidin- 1-yl）ethoxy）- 4H-chromen-4-one 3, was designed, prepared and structurally characterized by single-crystal X-ray diffraction. X-ray structure analysis reveals that 3 crystallizes in the orthorhombic system, space group Pbca, with a = 16.238（3）, b = 10.308（2）, c = 22.987（5）A, V = 3847.6（13）A3, Z = 8,μ= 0.093 mm^-1, Dc = 1.317 g/cm^3, F（000） = 1616, R = 0.0789 and wR = 0.1554 for 1463 observed reflections with I 〉 2σ（I）.     

微波辐射法合成丙二酸甲(乙)烷酯

丙二酸甲(乙)烷酯类是一些药物和天然产物合成的中间体,一般由丙二酸二甲(乙)酯经部分水解得到丙二酸单甲(乙)酯钠盐,再通过酸化、酰氯化和酯化反应制得[1],该方法路线较长、酰氯化反应会产生有毒尾气。羧酸(包括烷酸和芳酸)酯可由其盐和卤代烃直接反应制得[2-4],而且可利用无溶剂相转移催化的条件进一步加速反应和提高产率。微波技术用于有机合成[5-7]具有操作简便、产率高和速度快等优点。我们参考文献[2-4]方法,应用微波技术合成了标题化合物。1　实验部分1 1　仪器ＢｒｕｋｅｒＤＰＸ 300ＦＴ ＮＭＲ型核磁光谱仪,ＴＭＳ为内标;ＩＲ…     

Synthesis of Chiral N-Ferrocenylmethylaminoalcohols and their Application in Enantioselective Addition of Diethylzinc to Aldehydes

Three chiral N-ferrocenylmethylaminoalcohols were synthesized from readily available natural L-valine, leucine and phenylanine, and used as chiral ligands in the enantioselective addition of diethylzinc to aldehydes.     

基于联苯四羧酸的Zn(Ⅱ)配合物的合成、结构和性质

利用联苯四羧酸(H₄bptc)和双三唑乙烷(bte)合成了2个配位聚合物{[Zn₂(bptc)(DMF)₂(H₂O)]·DMF·H₂O}_n (1)和{[Zn(bte)(bptc)_0.5]·DMF·0.5H₂O}_n(2).化合物1为三维PtS-拓扑结构,在该配合物中每个双核次级构筑单元(SBU){Zn₂(O₂CR)₄}与4个联苯四酸配体相连,从而将配合物构筑成了三维MOF结构.化合物 2 为二维梯形结构,并通过弱氢键O…H-C将二维层连接为三维结构.同时对配合物的热稳定性和荧光特征进行了讨论.     

溴乙烷消去反应不宜采用演示实验进行教学

针对中学化学溴乙烷消去反应演示实验教学存在实验条件下反应复杂、演示实验反应方程式的表达与事实不符、实验现象易误导学生3个方面的问题,阐述了由于中学生思维方式和知识水平的局限,中学化学中溴乙烷消去反应内容的教学不宜采用演示实验。     

气相色谱-质谱/选择离子监测法用于苯乙烯不对称环氧化反应的筛选（英文）

建立了苯乙烯不对称环氧化反应的气相色谱-质谱/选择离子监测(GC-MS/SIM)筛选方法。以乙苯为内标,利用GC-MS/SIM对苯乙烯环氧化反应样品进行分析,在选定的分析条件下完全分离并准确测定了苯乙烯和环氧苯乙烷对映异构体的含量,同时利用该方法对苯乙烯环氧化反应的正交试验进行了评估。该方法具有以下优点:高精密度(以RSD表示的精密度为12%~52%,n=5)、良好的线性关系(苯乙烯、(R)-环氧苯乙烷和(S)-环氧苯乙烷标准曲线的相关系数分别为0999 7、0993 2和0996 3)、低定量限(苯乙烯、(R)-环氧苯乙烷和(S)-环氧苯乙烷的定量限分别为13、11和07 mg/L)以及合理的回收率(982%~1082%)。该方法为苯乙烯及其同系物的不对称环氧化反应提供了一种新的分析测定途径。     

Selective oxidation of ethane to aldehydes over SBA-15 supported molybdenum catalyst

SBA-15 supported Mo catalysts （Moy/SBA-15） were prepared by an ultrasonic assisted incipient-wetness impregnation method. The physical and chemical properties of the catalysts were characterized by means of N2-adsorption-desorption, XRD, TEM, UV-Vis, Raman, XANES and H2-TPR. The results showed that a trace amount of MoO3 was produced on high Mo content samples. Tum-over frequency （TOF） and product selectivity are dependent on the molybdenum content. Both Mo0.75/SBA-15 and Mo1.75/SBA-15 catalysts give the higher catalytic activity and the selectivity to the total aldehydes for the selective oxidation of C2H6. At the reaction temperature of 625℃, the maximum yield of aldehydes reached 4.2% over Mo0.75/SBA-15 catalyst. The improvement of the activity and selectivity was related with the state of MoOx species.     

ESTIMATION OF ACTIVATED ENERGY OF DESORPTION OF n—HEXANE ON ACTIVATED CARBONS BY PTD TECHNIQUE

In this paper,six kinds of activated carbons such as Ag^+-activated carbon,Cu^2+activated carbon,Fe^3+-activated carbon,activated carbon,Ba^2+-activated carbon and Ca^2+activated carbon were prepared.The model for estimating activated energy of desorption was established.Temperature-programmed desorption(TPD)experiments were conducted to measure the TPD curves of n-hexanol and then estimate the activation energy for desorption of n-hexanol on the activated carbons.Results showed that the activation energy for the desorption of n-hexanol on the Ag^+-activated carbon,the Cu^2+-activated carbon and the Fe^3+-activated carbon were higher than those of n-hexanol on the activated carbon,the Ca^2+-activated carbon and the Ba^2+-activated carbon.     

一种顶空气相色谱测定乳液聚合过程单体转化率的新方法

介绍了一种通过顶空气相色谱技术测定乳液聚合过程中单体转化率的新方法.通过对聚合乳液样品进行称量方式的采样和大比例的稀释,将已稀释的待测溶液移入顶空瓶中,在设定温度下达到气液平衡后进入气相色谱中测定,其消除了采样的波动性和顶空气相色谱测定的误差,并导出了由顶空气相色谱对样品中单体的测定信号直接计算聚合过程转化率的方程式.该方法具有实验操作简单、快速、检测准确等优点,非常适合乳液聚合反应动力学和机理的研究.     

钯与苯基羧酸和1,2—二（二苯膦）乙烷混配合物的合成与表征

合成得到钯与苯基羧酸和１，２－二９二苯磷）乙烷配位的四种混配配合物，确定其化学组成为Ｐｄ（ＰＣＡ）２（ｄｐｐｅ）。用元素分析，红外、紫外和荧光光谱、摩尔电导、质子核磁共振和热重分析等手段对配合物进行了性质表征。