2-羟基-1O,11-二氢-5H-二苯并[a,d]环庚烯-5-酮的合成

以2－羟基苯甲醛和3－甲氧基苯乙酸为原料,经3步反应合成2－羟基－10,11－二氢－5H－二苯并[a,d]环庚烯－5－酮。     

1-叠氮-2-苯并[f]茚满醇的四个光学活性异构体的合成

以1-苯并[f]茚为原料,合成了反式外消旋体1-叠氮-2-苯并[f]茚满醇[(±)-trans-1];(±)-trans-1经脂肪酶催化拆分得到两个反式对映异构体(1a和1c);1a和1c通过Mitsunobu反应构型转化得到两个顺式异构体(1b和1d).其结构经1H NMR和13C NMR表征;4个光学活性异构体1a～1d的光学纯度均为99%e.e..     

1-苯基-2-氰基-3-氨基-3a,3b,6,7-四氢化苯并[4,5]茚的合成及晶体结构

标题化合物C_20H_18N_2是由2-氰-3-苯基-3-(1-萘酮-2-基)丙腈在低价钛试剂作用下还原成环而得。结构通过单晶X-射线衍射分析确定,其晶体属于三斜晶系,空间群P, a = 9.169(2), b = 9.520(2), c = 10.276(2) , a = 91.09(1), = 107.95(1), = 111.05(2), V = 787.8(3),Mr = 286.36 ?, Dc = 1.207 g/cm3, Z = 2, m(MoKa) = 0.071 mm-1, F(000) = 304, R = 0.0399, wR = 0.1008。单晶X-射线分析表明,五员环(C(7)~C(11))采用信封式构象,而六员环(C(10)~C(15))则采用半椅式构象,同时,分子间氢键作用形成二聚体。     

4,5二氢[1,2,4]三氮唑并[4-3-a]喹林衍生物的合成

为了寻找正性肌力作用更强、副作用较小的治疗充血性心力衰竭的正性肌力药物 ,本文参照有关二氢喹啉酮类化合物的结构与正性肌力活性的文献报道[1- 5] ,在喹啉环上并入三氮唑 ,设计合成了 4,5二氢 [1 ,2 ,4]三氮唑并 [4 3 ａ]喹啉衍生物 ,以进一步探索二氢喹啉酮并入三唑环对其活性的影响。其结构经质谱、红外光谱和核磁共振氢谱表征。1　合成路线以苯胺为起始原料 ,经酰化、环合、硝化、还原、硫代、环合得 6 氨基 4,5二氢 [1 ,2 ,4]三氮唑并 [4 3 ａ]喹啉衍生物 :2　实验部分熔点用毛细管法测定 ,温度计未校正。红外光谱仪为ＦＴ ＩＲ1 …     

微波固相合成苯并[a]吩噁嗪衍生物

首次在固相条件下微波辐射N,N-二烷基-4-亚硝基苯胺盐酸盐和2-萘酚衍生物快速合成苯并[a]吩嗪衍生物,得到苯并[a]吩嗪离子氯化物3a-3f,且收率较高.此外,N,N-二甲基-4-亚硝基苯胺盐酸盐和1,3-二羟基-2-萘甲酸乙酯的混合物在微波辐射下合成了一个新的激光染料9-二甲氨基-6-乙氧羰基-5H-苯并[a]的吩 嗪-5-酮4.     

离子液体中一步合成14-芳基-1,6,7,14-四氢二苯并[a, i]吖啶-1,6-二酮衍生物

室温条件下在离子液体[bmim]BF4中合成了14-芳基-1,6,7,14-四氢二苯并[a, i]吖啶-1,6-二酮类衍生物,该方法具有产率高,反应介质可回收使用,反应底物范围广,反应时间短,操作简单等优点。     

氨基磺酸催化下三组分一锅法无溶剂合成苯并[4,5]咪唑并[1,2-a]嘧啶类衍生物

无溶剂条件下,用氨基磺酸催化芳香醛,2-氨基苯并咪唑和β-二羰基化合物的三组分反应,简单而方便地得到了苯并[4,5]咪唑并[1,2-a]嘧啶类衍生物.该法具有产率高,成本低廉,环境友好,适应性广简捷方便等优点.     

1a,3-二苯基-1,1,4,4-四氯-1a,2,3,4-四氢-1H-吖丙啶并[2,1-e][1,6]苯并硫氮杂辛因的合成及晶体结构

苯并杂类化合物为常用镇静剂及治疗心血管疾病和抗病毒的药物［１～３］,苯并杂与五六元杂环并合形成的三环化合物也是重要的药用杂环化合物,如１,４－苯并二氮杂与１,２,４－三唑并合形成的三环化合物为常用的治疗中枢神经系统疾病药物［４］．而吖丙啶与１,...     

区域选择性合成二苯并[d,f][1,3]二噁烷

针对二苯并[d,f][1,3]二噁烷传统制备方法中易产生二羟基联苯乙烯副产物的缺点,本文以路易斯酸性胍盐离子液体为催化剂,2,2'-二羟基联苯和端基炔为原料,高区域选择性的合成了二苯并[d,f][1,3]二噁烷,收率39%~84%。 本方法适用于各种端基炔。路易斯酸性胍盐离子液体循环利用5次,活性不变。     

新型三环系稠杂环[1,2,4]-三唑并[1,5-a][1]-苯并氮杂及[1,2,4]-三唑并[1,5-a]-喹啉的合成

α-四氢萘酮的乙氧羰基腙(1)经LTA氧化,得到α-偶氮-α-乙酰氧基化合物2.在A lC l3作用下,化合物2脱去乙酰氧基产生重氮正离子中间体3,再经与腈的1,3-偶极环加成、[1,2]-迁移扩环、碱性水解和与苦味酸作用,得到新型[1,2,4]-三唑并[1,5-a][1]苯并氮杂苦味酸盐6a~6c.以2,3-二氢-1-茚酮为底物,采用相同的合成路线,合成了1,2,4-三唑并[1,5-a]-二氢喹啉苦味酸盐12a~12c.     

Synthesis and characterization of a new pillar[5]arene-based [1]rotaxane

In this study, we reported the synthesis of three kinds of mono-functional pillar[5]arene derivatives PRI, PRII and R and their structures were studied by 1D and 2D NMR spectra and mass spectra. The 2D NMR spectra including ¹H-¹³C HSQC, ¹H-¹H COSY and NOESY spectra indicated that PRI and PRII are both stable self-included pseudo[1]rotaxanes in CDCl₃. These original structures are promising compounds for the design of pillar[5]-based [1]rotaxane. And the results showed that R could exist stable in CDCl₃ and DMSO because of the coordination of N-H?O hydrogen bonding interaction and C-H?π interaction.     

Synthesis of some 5H-benzo[a]phenothiazin-5-one derivatives

Several substituted 6-anilino-5H-benzo[a]phenothiazin-5-one derivatives were prepared by condensation of substituted 1,4-naphthoquinones with 2-aminobenzenethiol in pyridine. The reduction and acetylation of the resulting compounds were also investigated.

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Synthese einiger 5H-Benzo[a]phenothiazin-5-on-Derivate

Zusammenfassung Es wurden mittels Kondensation substituierter 1,4-Naphthochinone mit 2-Aminothiophenol in Pyridin einige substituierte 6-Anilino-5H-benzo[a]phenothiazin-5-one dargestellt. Die Reduktion und Acetylierung der resultierenden Verbindungen wurde ebenfalls untersucht.

     

Improved Synthesis of 9- and 10-Methylbenz[a] Anthracenes

The synthesis of 9- and 10-methylbenz[a]anthracenes by improved methods are described. These new procedures are simple and convenient, and provide the title compounds in good yields and high purity.     

A Facile Method for the Synthesis of 4- Acetylaminobenzo[15]crown-5

The 4-acetylaminobenzo[15]crown-5 is an important intermediate in the synthesis of crown ether cyanine dyes1, in addition, the acetylamino can easily be hydrolyzed to be amine2, to our knowledge which also is an usful intermediate3,4, The classical procedure for the synthesis of 4-acetylaminobenzo[15]crown-5 involves several steps2,5: typically nitration of the benzo[15]crown-5, followed by reduction of the introduced nitro group to form amine, and finally, acylation of the amine to give the am…     

稀土(Ⅲ)-三氟乙酰丙酮-4-皮考林-N-氧化物混配配合物的合成与表征

首次合成了稀土（Ⅲ）- 三氟乙酰丙酮（TFA）－4－皮考林－N－氧化物（4－picNO)混配配合物,通过元素分析确定其组成为Ln(TFA)2(3-picNO)(Ln=La,Nd,Eu,Tb),通过电导率,紫外光谱,IR和荧光光谱的测试,讨论了它们的性质。     

Synthesis of Several 2-Azafluorenones and 5H[1]Benzopyrano[3,4-c]Py Riding-Ones

Convenient syntheses of 2-azafluorenones 5a-f and 5H[1]benzopyrano[3,4-c]pyridin-5-ones 6a-b were performed by using intramolecular cyclization of 4-arylnicotinic acids 4a-F. 4a-f were obtained via permanganate oxidation from the corresponding of 4-arylpyridines 3a-f in good yields.     

Synthesis and Crystal Structure of 1-（4-Fluorophenyl）-2-hexylthiobenzo[4,5]-furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H）-one

The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5) ,β = 99.364(2) °,V = 4332.58(18) 3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I > 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.     

Synthesis and characterization of bis-[1]rotaxanes via salen-bridged bis-pillar[5]arenes

The series of salen-bridged bis-pillar[1]arenes were conveniently prepared by condensation reaction of5,5'-methylenebis(2-hydroxybenzalde hyde)or 5,5'-(propane-2,2-diyl)bis(2-hydroxybenzaldehyde)with mono-amido-functionalized pillar[5]arenes containing different terminal aminoalkyl groups in refluxing ethanol.The^1H NMR and 2D-NOESY spectra indicated that the salen-bridged bis-pillar[5]arenes with longer allcylene linker(n=3,4,6)formed the fascinating bis-[1]rotaxanes,while the salenbridged bis-pillar[5]arenes with short hydrazine and ethylenediamino linker(n=0,2)predominately existed in free form.The single crystal structure of the bis-pillar[5]are ne ambiguously indicated that two propylenediamino linker inserted in to two cavities of pillar[5]arene to form a novel bis-[1]rotaxanes.     

Metal(II) Complexes Based on Imidazo[4, 5‐f]‐1, 10‐phenanthroline and Bridging Dicarboxylato Ligands: Synthesis,Characterization and Photoluminescence

Eight metal(II) complexes based on imidazo[4, 5‐f]‐1, 10‐phenanthroline (HIMP) and bridging dicarboxylato ligands such as 4, 4′‐biphenyldicarboxylic acid (H₂BPDC), 1, 4‐benzenedicarboxylic acid (H₂BDC), thiophene‐2, 5‐dicarboxylic acid (H₂TDC), and 2, 6‐naphthalenedicarboxylic acid (H₂NDC) were hydrothermally synthesized and structurally characterized by single‐crystal X‐ray diffraction. Complexes 1 , 3 , 6 , and 7 are molecular dinuclear metal complexes. Complexes 2 , 4 , and 5 exhibit chain‐like structures. Compound 8 shows a novel 3D architecture, in which Zn^II dimers are connected by four NDC^2– anions. In the metal(II) complexes, HIMP exhibits a similar chelating coordination mode. Different π ··· π stacking interactions are observed in the complexes. The emission of HIMP is completely quenched in complexes 1 – 4 due to the strong π ··· π stacking interactions in the structures. Complexes 5 – 8 exhibit different photoluminescence properties. Firstly, we quantitatively investigated the effect of the strong HIMP–HIMP stacking interactions on the emission quenching of HIMP in the metal complexes. It was found that a higher extent of π ··· π stacking interactions in the complexes resulted in a higher extent of the emission quenching of HIMP. The introduction of aromatic conjugated carboxylate groups into metal(II)‐HIMP complexes changed the extent of the strong π ··· π stacking interactions in the structures and thus the photoluminescence properties of the complexes.