双N—乙酸取代氮氧杂大环及其镧系配合物的合成

首次合成了一种新的1.2-双(3,4:9,10-二苯并-5,8-二氧杂-1,12-二氮杂环十五烷-N-乙酸)乙烷大环配体,制备了它的8个镧系元素(La,Pr,Nd,Sm,EU,Gd,Dy,Yb)配合物,用红外光谱、元素分析、核磁共振谱及电导等方法进行了表征,讨论了可能的配位情况。     

Synthesis of mesoionic[1,2,3]triazolo[5,1-d][1,2,5]triazepines

Intramolecular cyclization of 1-amino-3-phenacyl-4-carbohydrazido-1,2,3-triazolium-5-olates has been shown to take place via selective interaction of the carbonyl group with the terminal amino function of the hydrazido group to form a 1,2,5-triazepine ring. Minor products, resulting from the interaction of the α-nitrogen atom of the hydrazido group with the carbonyl function, having a N-amino-pyridazine structure were also detected and isolated. A general method for the synthesis of novel mesoionic 2-amino-7-aryl-4-oxo-2,4,5,8-tetrahydro[1,2,3]triazolo[5,1-d][1,2,5]triazepin-9-ium-3-olates was developed.     

Synthesis and properties of substituted 2-methylene-hydrazono-2,3-dihydro-3-benzo[<Emphasis Type="Italic">b</Emphasis>]furanones

The reaction of 2,3-dihydro-2,3-benzo[b]furandione with the triphenylphosphazines of diazo compounds leads to substituted 2-methylenehydrazono-2,3-dihydro-3-benzo[b]furanones, which are hydrolyzed in an acidic medium to the substituted methylenehydrazides of o-hydroxyphenylglyoxalic acid and react with amines to form the products of addition at the activated CH=N bond of the side chain or 2-hydrazono-2,3-dihydro-3-benzo[b]furanone respectively. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 817–822, June, 2007.     

取代乙酸配体对乙炔二聚反应催化剂性能的影响

研究了取代乙酸配体作为Ｎｉｅｕｌａｎ催化剂对乙炔二聚反应性能的影响。结果表明，不同功能结构数目的影响，结果表明，不同功能结构数目的的氨羧配体均使催化剂的选择性提高。乙炔转化率略有下降，巯基乙酸配体的加入，则改变了乙炔二聚反应的机理，得到以乙醛为主的产物。     

取代肉桂酰甘氨酸酯的合成

在N-甲基吡咯烷酮(NMP)促进下,取代肉桂酸(1a^1g)与二氯亚砜(SOCl2)在20℃酰氯化反应0.5 h,再加入甘氨酸乙酯盐酸盐,在40℃下酰胺化反应4 h,n(取代肉桂酸)/n(SOCl2)/n(甘氨酸乙酯盐酸盐)=1.0/1.2/1.4,合成了一系列取代肉桂酰甘氨酸乙酯(2a^2g),其结构经1H NMR、13C NMR、IR和MS(EI)确证。并探讨了NMP促进取代肉桂酰甘氨酸乙酯反应可能的机理。     

2,4—二氨基—5—取代苄基嘧啶类质谱研究

报道了8个2,4-二氨基-5-取代苄基嘧啶衍生物的电子轰击质谱及碰撞活化解离和质量分析离子动能谱.该谱提供了化合物醚键及2,4-二氨基-5-取代苄基嘧啶环的主要碎裂途径,总结了一些裂解规律,将有助于这类化合物的结构推断。     

Highly Efficient One-Pot Synthesis of 2-Arylmethyl N-Substituted Anilines via Yb（OTf）3 Catalyzed Three-Component Reaction

An efficient method has been developed for one-pot three-component coupling reactions of various aldehydes, 1-cyclohexen-2-one, and primary or secondary amines in the presence of a catalytic amount of Yb（OTf）3 under mild conditions to afford the corresponding 2-arylmethyl N-substituted anilines in good yields. In addition, the catalyst was easily recovered and could be reused for at least four cycles without any loss of activity.     

苯胺类化合物的电化学氧化及随后化学反应

利用循环伏安法研究了二取代对苯二胺(1),四取代对苯二胺(2)和二取代氨基酚(3)三类化合物以及它们的衍生物的电化学行为及其氧化产物的随后不可逆脱氨反应。 1类化合物在任何pH下的电化学氧化均为一步双电子转移反应,2类化合物为二步单电子转移反应;3类化合物在酸性和中性范围为一步双电子氧化在碱性溶液中为二步单电子转移反应。文中定量求算了不可逆随后化学反应的表观水解速率常数k_f,并进行了讨论。     

Cyanosilylation of α-butylthioacrolein

Cyanosilylation of α-butylthioacrolein with trimethylsilyl cyanide occurs as 1,2-addition. Concurrent rapid dimerization of α-butylthioacrolein occurred both in the presence and in the absence of H₂PtCl₆·6H₂O as a catalyst to give 2,5-dibutylthio-2,3-dihydro-4H-pyran-2-carbaldehyde, whose cyanosilylation afforded the corresponding cyanohydrin. The latter is prone to retrodiene degradation upon heating. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1418–1420, July, 1998.     

Synthesis of substituted polymethylenes by radical polymerization of alkyl N,N-dialkylfumaramates and maleamates: Relative reactivity of the isomers

Bulk polymerization of alkyl N,N-dialkylfumaramates (FAE) and maleamates (MAE) was performed in the presence of a radical initiator. It has been found that FAE is more reactive than MAE when the reactivity of the two geometrical isomers was compared for their homo- and copolymerizations. From investigation on the effect of ester and N-substituents of these monomers, it has been found that the isopropyl ester shows a higher reactivity than the methyl ester and that N-ethyl and n-butyl substitution gives polymers with high molecular weight of more than several thousands. The resulting substituted polymethylenes from FAE and MAE were characterized and compared with each other. The isomerization of MAE to FAE with morpholine as an isomerization catalyst and monomer-isomerization radical polymerization were also investigated.