溶胶-凝胶法制备铁酸盐超微粒子催化剂

采用溶胶－凝胶法制备了含Zn,Ni,Co的铁酸盐超微粒子催化剂，运用DTA－TG、IR、XRD以及BET比表面测试等手段对所制备的样品进行了表征。同时，考察了铁酸盐对二氧化碳选择性氧化乙苯制苯乙烯的催化性能。结果表明：制备的铁酸盐均为尖晶石型晶体，粒子的比表面积为31．9－36．3m^2/g，晶粒大小约为30－35nm，在由二氧化碳选择性氧化乙苯制苯乙烯的反应中表现出较好的催化活性。     

芳亚甲基丙二腈、芳亚甲基氰乙酰胺的固相合成

芳醛和丙二腈、氰乙酰胺在NH4Ac催化下经固相反应高产率的得到芳亚甲基丙 二腈和芳亚甲基氰乙酰胺。     

Facile cyclic ammonium salt with the smallest size for high performance electric double layer capacitors

A novel cyclic ammonium salt, N,N-dimethylpyrrolidinium tetrafluoroborate (P₁₁-BF₄), was successfully synthesized for the first time. The smallest cyclic structure of P₁₁-BF₄ induced high solubility and conductivity in PC, which can easier enter the micropores of activated carbon and occupy more surface area during charge/discharge process.     

Tree-gel and loop-gel conversions in nonlinear polymerization

Ａｓｉｓｗｅｌｌｋｎｏｗｎ,ｔｈｅｔｈｅｏｒｙｆｏｒｎｏｎｌｉｎｅａｒｐｏｌｙｍｅｒｉｚａｔｉｏｎｓｗａｓｉｎｉｔｉａｔｅｄｂｙＦｌｏｒｙａｎｄＳｔｏｃｋｍａｙｅｒ[1—3].ＭｉｌｌｅｒａｎｄＭａｃｏｓｋｏ[4—6]ｐｒｏｐｏｓｅｄａｒｅｃｕｒｓｉｖｅｍｅｔｈｏｄｆｏｒｄｅａｌｉｎｇｗｉｔｈｔｈｅｐｒｏｂｌｅｍｏｆｔｈｅｐｏｓｔｇｅｌｐｒｏｐｅｒｔｉｅｓｏｆｔｈｅｎｅｔｗｏｒｋｆｏｒｍｉｎｇｐｏｌｙｍｅｒｉｚａｔｉｏｎ.Ｓｔｅｐｔｏ[7]ｉｎｖｅｓｔｉｇａｔｅｄｔｈｅｇｅｌｇｅｌｒｅａｃｔｉｏｎｏｆＲＡｆｔ…     

Michael Addition of Thiols to á,(a)-Unsaturated Carbonyl Compounds Catalyzed by Bifunctional Organocatalysts:Asymmetric Michael Addition and Asymmetric Protonation

Recently the hydrogen-bond activated reactions have attracted much attention.1 Takemoto2 reported a highly enantioselective Michael addition of manolate to nitroolefins catalyzed by a bifunctional organocatalyst with tertiary amine and thiourea moiety. As we known,stereoselective conjugate additions of thiols are interesting due to the standpoint of biological and synthetic importance, however, only very limited good results have been obtained except for the works of Shibasaki3, Kanemasa4 and Deng5 et al.In this letter, we report an efficient catalytic asymmetric Michael reactions of thiols to a,a-unsaturated carbonyl compounds promoted by bifunctional organocatalysts. A series of organocatalysts with chiral amine and thiourea structures were designed and synthesized and have been successfully applied in the conjugated additions of thiols to a,a-unsaturated imides and enones.The reactions got quantitative yields and the ee values were up to 84%. It is noteworthy that the a-asymmetric protonation (up to 43% ee) also could be achieved.The Michael addition between aromatic thiols and a,a-unsaturated carbonyl compounds isdescribed as follows:Works to further increase the enantioselectivity is under investigation in our laboratory.     

Diastereoselective Three Component Reaction of N‐Glyoxyloyl Camphorpyrazolidinone,Amine and Allyltributylstannane: Facile Synthesis of Homoallylic Amines

Diastereoselective allylation of imine derived from N‐glyoxyloyl camphorpyrazolidinone and amines was treated with allyltributylstannane in the presence of triflic acid. The corresponding optically enriched homoallylic amines were obtained in reasonable to high material yields and with practical levels of stereoselectivity in 10 min at ambient temperature.     

超声条件下溶胶-凝胶法制备CaSiO_3∶(Pb,Mn)发光材料的研究

采用溶胶-凝胶法并辅以超声技术制备了CaSiO3∶(Pb,Mn)发光材料,对合成物运用荧光光谱、DTA-TG、XRD、FTIR、TEM等手段进行了表征。研究了制备时的物料配比、超声时间及焙烧温度对样品发光强度的影响,找到了最佳的合成条件。结果表明,所得样品其荧光强度约为高温固相法样品的2倍,平均粒径则降低约300 nm。     

Selective dimerization of α-methylstyrene catalyzed by a solid acid

A novel solid acid prepared from concentrated sulfuric, boric and phosphoric acid is a highly selective catalyst for the dimerization of α-methylstyrene at room temperature to generate 4-methyl-2,4-diphenyl-1-pentene.     

Studies on the Spectral Behavior between Protein with Poniacyl Carmine 2B and its Analytical Application

In this paper, the spectral behavior of protein and Poniacyl Carmine 2B (PC 2B) has been studied by spectrophotometric method. The conditional constants, apparent combination constant K and maximum binding number n, were used to express the combination ability of the reactions between PC 2B and protein under a set of given conditions. The Sandell index s was used to express the sensitivity of the determination of protein. The factors, acidity, PC 2B concentration and the ionic strength, were discussed by the change of apparent combination constant and maximum binding number. It was found that acidity of the solution, PC 2B concentration and ionic strength had a significant effect on the sensitivity of the assay of protein. Under the optimal conditions, the apparent combination constant K and the maximum binding number n were 2.36 × 10⁶ L mol^?1 and 95, respectively. With further investigation, it was found that the Scatchard model was suitable in treating the data obtained in the experiments. In the buffer medium of HCl‐KCl at 1.87, the addition of protein made the maximum absorption of the system move from 527 nm to 513 nm. Its apparent molar absorptivity is 4.46 × 10⁵ Lmol^?1 cm^?1 at 513 nm. Beer's law is obeyed in the range of 0 ? 55 μg mL^?1. The system developed in this paper has been used for the determination of protein in milk powder successfully.     

Total synthesis of a conformationally constrained didemnin B analog

The total synthesis of a didemnin B analogue containing a conformationally constrained replacement for the isostatine moiety is reported. Synthetic highlights include an improved preparation of 2-hydroxy-3-cyclohexenecarboxylic acid and a new strategy for accessing the macrocycle.