一种吲哚螺吡啶并嘧啶杂环衍生物的合成及其晶体结构

利用多组分反应方法,合成了一种螺环结构的2′,7′-二氨基-5-甲基-2,4′-二氧代-4′,8′-二氢-3’H-螺[吲哚啉-3,5′-吡啶[2,3-d]嘧啶]-6′-腈化合物4,并对该化合物进行了红外光谱、核磁共振氢谱、元素分析以及X-射线单晶衍射表征.单晶衍射结果表明:该晶体属于三斜晶系,空间群P-1,晶体参数为a=1.308 1nm,b=1.316 3nm,c=1.454 2nm,α=71.668(1)°,β=78.074(2)°,γ=66.475(1)°.在每个晶胞结构单元中含有一对对映异构体分子,分子中通过螺碳原子相连的吲哚环和二氢吡啶环处于几乎垂直构型,其二面角为89.15(2)°;稠合的二氢吡啶环和嘧啶环几乎共平面,其二面角为0.93(2)°.     

两个三环己基锡芳香羧酸酯的合成、结构、热稳定性及体外抗癌活性研究

甲醇中三环己基氢氧化锡分别与呋喃-2-甲酸、2,4,6-三甲基苯甲酸反应,合成了2个三环己基锡芳香羧酸酯Cy3SnO2CC4H3O(1)和Cy3SnO2CC6H2Me3(2)(Cy为环己基)。通过IR、1H和13C NMR、元素分析及X-射线单晶衍射表征结构。1和2均属单斜晶系,配合物1空间群P21,晶体学参数:a=0.823 04(2)nm,b=1.111 19(3)nm,c=1.283 90(3)nm,β=101.090(2)°,Z=2,V=1.152 27(5)nm3,Dc=1.381 g·cm-3,μ(Mo Kα)=1.127 mm-1,F(000)=496,R1=0.052 9,wR2=0.138 7。配合物2空间群P21/c,晶体学参数:a=0.999 62(2)nm,b=1.415 97(2)nm,c=1.973 59(3)nm,β=94.042 0(10)°,Z=4,V=2.786 53(8)nm3,Dc=1.266 g·cm-3,μ(Mo Kα)=0.937 mm-1,F(000)=1 112,R1=0.0540,wR2=0.161 9。配合物(1)和(2)的中心锡原子均为畸变四面体构型。通过分子间氢键作用,配合物(1)形成二维网状结构。试验表明,配合物1和2具有良好的热稳定性,对人癌细胞Colo205、HepG2、MCF-7、Hela、NCI-H460增殖均有较强的抑制作用。     

光催化合成金属Ag纳米颗粒的生长机制——晶核密度控制的生长模式转换

利用AgNO3水溶液,通过严格控制TiO2薄膜的化学活性,系统研究了在TiO2表面光催化合成金属Ag纳米颗粒的生长行为。研究发现,光催化合成金属Ag纳米颗粒存在着两个完全不同的生长机制,分别对应着金属Ag纳米颗粒的各向同性和各向异性生长。当溶液浓度较低时,Ostwald熟化(OR)机制主导着金属Ag纳米颗粒的长大过程;当溶液浓度较高时,取向附生(OA)机制决定着金属Ag纳米颗粒长大成纳米片。原位消光光谱分析表明,OR机制和OA机制生长的前期具有相近消光特征,决定金属Ag纳米颗粒生长模式的关键是AgNO3溶液的浓度,更准确地说是金属Ag初级晶核的局域密度。在此基础上提出了有关光催化合成金属Ag纳米颗粒的生长模型。     

4-氯苯氧乙酸和1,10-邻菲啰呤构筑的双核铽配合物的晶体结构,荧光和生物活性(英文)

水热条件下采用Tb(NO3)3·6(H2O),4-氯苯氧乙酸和1,10-邻菲啰呤作为反应物合成出1个双核铽配合物[Tb2(4-Hcpoa)5(phen)2(NO3)](1)(4-Hcpoa=4-氯苯氧乙酸,phen=1,10-邻菲啰呤),并分别用元素分析、红外光谱、差热分析、X-射线粉末衍射和X-射线单晶衍射等表征了该结构。晶体结构分析结果表明:2个双齿和2个三齿4-氯苯氧乙酸配体将2个铽金属离子连接成二聚体结构。荧光分析表明常温固态下配合物1发射绿色荧光,且在544 nm处的荧光寿命为0.920 ms。以除草剂精喹禾灵为对照品,研究了配体4-氯苯氧乙酸及其配合物1对甘蓝型油菜和钝芒稗的抑制作用。     

无机-有机杂化硫属化合物[Mn(1,2-dap)_2(H_2O)]_2(μ-Sn_2Q_6)(Q=S、Se)和[Mn(tren)]_2(μ-Sn_2S_6)的合成、晶体结构与性能（英文）

采用溶剂热方法合成了3个多元硫属化合物[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)(Q=S(1)和Se(2))和[Mn(tren)]2(μ-Sn2S6)(3),用X-射线单晶衍射测定了化合物的结构,并通过红外光谱、紫外-可见漫反射光谱对其进行了表征。单晶结构解析表明,化合物1和2都属于正交晶系,Pccn空间群(No.56),晶体结构是由[Mn(1,2-dap)2(H2O)]2+配合物阳离子和[Sn2Q6]4-二聚体通过Mn-Q键连接而成的[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)低聚体,相邻的低聚体之间通过氢键相连形成三维结构。化合物3属于三斜晶系,晶体结构是由[Mn(tren)]2(μ-Sn2S6)单元通过氢键连接而成的二维结构。紫外-可见漫反射光谱结果显示化合物1,2和3的带隙分别为2.5,2.1,2.4 e V,属于半导体材料。     

Synthesis and characterization of acetylated sept-D-glucopyranose carbamate as an oligosaccharide donor简

An oligosaccharide donor, acetylated sept-o-glucopyranose tetradecyl carbamate, was designed and synthesized. This compound could be easily linked to hydroxyl-containing compounds through an Oglycosidic bond. Characterization of all the oligosaccharide intermediates and the final product was thoroughly discussed.     

Synthesis and acaricidal activity of strobilurin-pyrimidine derivatives简

Pyriminostrobin, a new acaricide, was discovered in our previous studies. Because introducing fluorine into organic compounds can increase bioactivity, pyriminostrobin was modified as a series of strobilurin-pyrimidine derivatives for biological screening. The compounds were characterized by 1H NMR, MS and elemental analysis. Preliminary bioassays demonstrated that compounds 7e and 7i exhibited significant control against Tetranychus cinnabarinus （Boisd.） at 0.625 mg L^-1, and their acaricidal potencies were higher than pyriminostrobin in a greenhouse. The relationship between structure and acaricidal activity was also studied.     

Propane-1,2,3-triyl tris(hydrogen sulfate): A mild and effcient recyclable catalyst for the synthesis of biscoumarin derivatives in water and solvent-free conditions简

A simple, efficient, and ecofriendly procedure has been developed using propane-l,2,3-triyl tris（hydrogen sulfate） as a catalyst for the synthesis of biscoumarin derivatives in water and solvent-free conditions. The significant features of the present protocol are simplicity, environmentally benign, high yields, no chromatographic separation, and recyclability of the catalyst.     

2-羰基丙酸(芳甲酰基)腙二(2,4-二氯苄基)锡配合物的合成、晶体结构、热稳定性及与DNA相互作用研究

在含水甲苯中,2,4-二氯苄与锡粉反应合成了二(2,4-二氯苄基)二氯化锡,将其分别与2-羰基丙酸(苯甲酰基)腙及2-羰基丙酸(水杨酰基)腙反应,合成了2个取代苄基锡配合物(C2、C3),配合物C2和C3通过元素分析、1H NMR、13C NMR、IR、UV-Vis等表征,运用X-射线单晶衍射测试了2个有机锡配合物的分子结构,结构分析表明,锡与配位原子形成变形五角双锥构型的双核有机锡配合物,分子以Sn2O2四元环为中心对称。热分析结果表明,在空气氛下,配合物C2在121℃、C3在128℃以下可稳定存在;在Tris-HCl缓冲溶液中,以EB做为荧光探针,用荧光光谱法初步研究了配合物与鲱鱼精DNA的相互作用,结果表明配合物与鲱鱼精DNA作用是插入结合与静电结合共同作用所致。     

Synthesis of cyclopentenyl and cyclohexenyl ketones via [3 + 2] and [4 + 2] annulations of 1,2-allenic ketones简

In this paper, an efficient synthesis of cyclopentenyl ketones and cyclohexenyl ketones through tertiary phosphine catalyzed [3 ＋ 2] and [4 ＋ 2] annulations of 1,2-allenic ketones with activated alkenes has been developed. Compared with published synthetic methods on cyclopentenyl ketones and cyclohexenyl ketones, the protocols developed in this paper have the advantages such as readily available starting materials, mild reaction conditions and high efficiency.