1-烷（苯）氧基-3-（3，4-亚甲基二氧）苯基-2-丙醇的合成与生物活性研究

黄樟素氧化物与烷氧基钠和苯氧基钠反应，区域选择性地开环加成，生成1-烷 （苯）氧基-3-（3，4-亚甲基二氧）苯基-2-丙醇。该系列化合物具有诱导细胞凋 亡与分化的生物活性。     

Synthesis and Electrospray Ionization Mass Spectra of N-（1,3, 2-Dioxaphosphorinan-2-ylmethyl）thiophosphoramidates

N-（1,3,2-Dioxaphosphorinan-2-ylmethyl）thiophosphoramidates were synthesized and determined by NMR spectra and positive ion electrospray ionization mass spectrometry （ESI-MS） in conjunction with tandem mass spectrometry （MS/MS）. The fragmentation pathways were investigated. The results show that these characteristic ions in ESI mass spectra are useful in the structural determination of N-（1,3,2-dioxaphosphorinan-2-ylmethyl）- thiophosphoramidates.     

SrTi0.9M0.1O3-δ钙钛矿型氧化物催化剂甲烷氧化偶联反应性能的研究

The structure and catalytic properties of SrTi_0.9M_0.1O_3-δ (M=Mg，Al， Zr) perovskite-type catalysts for ox-idative coupling of methane (OCM) have been studied by using X-ray diffraction (XRD)，X-ray photoelectron spectroscopy (XPS) and temperature-programmed desorption of oxygen(O₂-TPD) methods. It has been shown that doping the cations of lower valence (e.g. Mg²⁺， Al³⁺) to the B site of SrTi_0.9M_0.1O_3-δ perovskite-type catalysts results in the higher content of adsorbed oxygen species on the surface of catalysts and thus higher C₂-selectivity for OCM reaction. It is suggested that the oxygen vacancies of SrTi_0.9M_0.1O_3-δ (M=Mg， Al， Zr) perovskite-type catalysts are the sites responsible for oxygen activation， and the adsorbed oxygen species on the surface of SrTi_0.9M_0.1O_3-δ catalysts are the main active species for OCM reaction.     

Enantioselective Addition of Phenylacetylene to Aldehydes Catalyzed by Polymer-Supported Sulfonamide

Enantioselective formation of C-C bonds is an area of intense research. Among them, the asymmetric addition of alkynyl reagents to aldehydes is very useful for the synthesis of chiral secondary propargyl alcohols.[1] Recently, many significant homogeneous chiral ligands have been disclosed,[2,3] but very few efficient heterogeneous catalysts have been reported. Herein, we report our research results in the asymmetric addition of phenylacetylene to aldehydes catalyzed by polymer-supported chiral sulfonamide.     

7-(对甲酰基苯偶氮)-8-羟基喹啉-5-磺酸的合成及其双波长分光光度法测定镓

7－（对甲酰基苯偶氮）－8－羟基喹啉－5－磺酸是一新显色剂。该试剂在微碱性介质中（pH＝7．5）与镓形成黄色络合物。络合物λmax＝392nm，摩尔吸光系数ε392＝2．24×104L·mol-1·cm-1。同时在500nm呈现负峰，用双峰观波长法测定镓ε392～500＝6．89×104L·mol-1·cm－1，灵敏度是单波长法的三倍多．线性范围0～2．0×10－5mol／L。用拟定的方法测定了掺硅的GaAS材料及岩石中的镓，加入回收率为106％～110％；方法的相对标准偏差小于1．6％。     

选择性远程DEPT NMR技术用于萜类生物碱的结构测定

从中草药勒党根茎中分离出二个化合物, 其一为已知的萜类生物碱culamtraramine, 其二为它的差向立体异构体, 为新化合物, 定名为isoculantraramine。用选择性远程核磁共振技术测定了它们的结构。     

超声辐射下一步法合成2-氨基-3-氰基-4-芳基-7，7-二甲基-5-氧代-5，6，7，8-四氢-4H-苯并[b]吡喃

芳醛、丙二腈和5，5-二甲基-1，3-环己二酮在乙二醇中不加任何催化剂经超 声辐射5-7min得2-氨基-3-氰基-4-芳基-7，7-二甲基-5-氧代-4H-5，6，7，8-四氢 苯并[b]吡喃，产率88％—96％．     

影响面粉中铝含量测定因素分析

目的探讨了江苏省疾控[2009]97号文件附录A《面制品及海蜇中铝的测定方法》测定面制食品中铝含量。方法样品经干法消化后,在乙二胺-盐酸缓冲溶液中,三价铝在十六烷基三甲基溴化铵阳离子表面活性剂存在下,与铬天青S形成绿色三元体系,其吸光度与铝的含量在一定含量范围内成正比。结果样品消化液在定容30 min时测定结果接近中位值,方法线性系数r=0.999 7,相对标准偏差在3.3%~3.7%之间,样品回收率在88.9%~96.4%。结论该法操作简便,灵敏度高,适用于各实验室开展检测。     

σ2 Hessian方程的Pogorelov型C2 内估计及应用

提出利用拉格朗日乘子法重新证明σ2算子的最优凹性,并定义了一个凸锥Γ3?=λ=(λ1,λ2,?,λn)∈Rn:σ1(λ)>0,σ2(λ|i)>0,1≤i≤n。利用σ2算子的最优凹性，给出了σ2Hessian方程Pogorelov型C2内估计，进而证明了σ2(D2u(x))=1,x∈Rn的满足二次多项式增长条件的Γ3?-凸整解为二次多项式。     

含硫柔性二苯甲酸及氮杂环配体的Zn(Ⅱ)和Mn(Ⅱ)配合物的合成及晶体结构

以2,2'-二硫代二苯甲酸、2,2'-联吡啶、咪唑、硝酸锌和硝酸锰为原料,使用水热方法合成了配合物[Zn(EBLA)(2,2'-bipy)(H₂O)](EBLA=2,2'-二苯甲酸硫醚)(2,2'-bipy=2,2'-联吡啶)(1),自然挥发法制备了配合物[Mn(EBSA)(im)₂(H₂O)]_n(EBSA=2,2'-二硫代二苯甲酸)(im=咪唑)(2).利用元素分析、红外和热重分析对其进行了表征.利用X-射线单晶衍射对结构进行了测定,并研究了配合物1的荧光性质.配合物1中,2,2'-二苯甲酸硫醚是通过水热方法由2,2'-二硫代二苯甲酸发生原位反应制备,Zn²⁺离子是五配位的四角锥双核结构;配合物2中,Mn²⁺离子是六配位的变形八面体一维链状结构.配合物中存在氢键和π-π堆积等弱的分子间作用力.