Hypervalent Iodine(III) Sulfonate Mediated Synthesis of Imidazo[1,2‐a]pyridines

A direct and efficient method for the conversion of alkyl aryl ketones to imidazo[1,2‐α]pyridines has been developed based on initial formation of α‐organosulfonyloxy ketones and their subsequent cyclocondensation by 2‐aminopyridines in one‐pot conditions.     

呋喃甲醛缩二乙撑三胺希夫碱铜配合物的合成及结构(英)

A novel copper(Ⅱ) complex CuL(NO₃)₂(where L=N,N′-bis(furaldehyde)-diethylenetriamine) was synthesized and characterized by X-ray crystallography analysis. The crystal belongs to monoclinic, space group C2/c with cell parameters a=1.924 0(6) nm, b=0.792 8(3) nm, c=2.504 1(8) nm, β=111.163(5)°, and Z=8. The coordination geometry around Cu(Ⅱ) is a distorted trigonal-bipyramid，and one-dimensional chain is formed through intermolecular hydrogen bonds. CCDC: 255629.     

Solid state reactions of nitrogenous heterocyclic compounds(Ⅰ)——Solid state reactions of 3-methyl-l-phenyl-5-pyrazolone with carbonyl compounds

The solid state reaction of 3-methyl-1-phenyl-5-pyrazolone (MPP) with aromatic aldehydes and ke-tones benzil derivatives and imides,and the solid state Michael addition reaction of MPP with 4-arylidene-3-methyl-1-phenyl-5-pyrnzolone 2 were investigated.Some new solid state reactions between the reactants were found,from which a series of new compounds were obtained The structures of the products were identified by IR,1H NMR,MS,elemental analyses and also by X-ray crystal analysis,and the reaction mechanism of MPP with aromatic aldehydes and ketones was proposed     

Rh／SiO_2上H_2的化学吸附

Ｒｈ／ＳｉＯ_２上Ｈ_２的化学吸附陈耀强，龚茂初，明虹，周建略，杜宗英，祝小红，陈豫（四川大学化学系，成都，６１００６４）关键词Ｒｈ／ＳｉＯ_２催化剂，Ｈ_２化学吸附，ＩＲＨ２在Ｒｈ上的化学吸附被认为是解离化学吸附［１］．而Ｒｈ－Ｈ的红外振动谱带是Ｈ２在...     

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。     

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。     

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.