几种取代螺吲哚啉萘并噁嗪的合成

螺吲哚啉-2,3'-[3H]萘并[2,1-b][1,4]噁嗪(简称螺噁嗪)是一类耐光疲劳性能优于螺吡喃的光致变色物^[1]。Fox以及Ono先期合成了这类化合物^[2],最近Pottier等考察了取代基对性能的影响^[3,4]。但所涉及的取代基(CH₃、CH₃O、Cl、NO₂)多在母体结构中吲哚环的5( 6)位,且N-烷基碳链较短,蔡环上有取代基的情形较少见^[5]。     

SYNTHESIS AND PHOTOCYTOTOXICITY OF SOME NEW SUBSTITUTED PHTHALOCYANINES

Some new, ring-substituted phthalocyanines have been synthesized and underwent preliminary testing for photodynamic activity using the colony forming ability of Chinese hamster cells in culture as an endpoint. Using 4-(3-N,N-diethylaminopropyl)phthalonitrile as a precursor, the previously unknown metal-free 2,9,16,23-tetra-(3-N,N-diethylaminopropyl)phthalocyanine was prepared and converted to its zinc (II) and its cationic water-soluble 2,9,16,23-tetramethylammonium zinc (II) iodide derivatives. Other new phthalocyanine derivatives tested, include a 2,9,16,23-tetra(2-hydroxymethyl-2-methylbutoxy)phthalocyaninato zinc (II) and 2,3,9,10,16,17,23,24-octahydroxyphthalocyaninato zinc (II) derivatives. Boron tribromide cleavage of the newly prepared and fully characterized 2,3,9,10,16,17,23,24-octamethoxyphthalocyanine gave the unstable metal-free octahydroxyphthalocyanine, which could only be characterized by ultraviolet-visible, NMR and IR spectroscopy.     

取代芳甲酰哌嗪新衍生物的合成及其药理活性

１引言充血性心力衰竭是目前临床上较为常见的心血管系统疾病之一，由其引起的死亡率在不断增加。维司力农（Ｖｅｓｎａｒｉｏｎｅ，ＯＰＣ－８２１２，Ｉ）作为正性肌力药于１９９０年首先在日本上市，其正性肌力作用选择性高，无明显变时效应和血管作用。但该化合物结构复杂，合成路线较长且安全范围较窄［’１。本课题组以维司力农为模型化合物，将其结构改造，得到一系列３，４一二甲氧基苯甲酸听唤衍生物，药理试验表明具一定的正性肌力作用出。在此基础上，作者设计以吹哺甲酸基及（取代）苯甲酸基代替３，４一二甲氧基苯甲酚基，合成…     

烷基取代聚对亚苯基亚乙烯基衍生物的合成和性质研究

设计了一种合成烷基取代聚对苯撑乙烯 (PPV)衍生物的新方法 ,合成了一种新的烷基取代PPV 聚(2 甲基 5 十二烷基对苯撑乙烯 ) ,并用NMR、IR、GPC、元素分析等方法对化合物进行了表征与鉴定 .同时 ,测试了化合物的热学性质、紫外可见吸收和光致荧光性质 .发现化合物的玻璃化温度和第一分解温度随着共轭程度的增加而升高 ;化合物的THF稀溶液的光致荧光相对量子产率随共轭程度的降低而增加     

SYNTHESIS OF SOME BICYCLIC THIAZOLO AND THIAZEPINOPYRIMIDINE DERIVATIVES

Thiazolo 3 a–c and oxothialo 5 a–b pyrimidine compounds were synthesized by a simple one-pot condensation reaction of the pyrimidine derivative i 1a and 1,2-dibromoethane i 2 or 2-bromopropanoic acid 4 . In a similar way the thiazepinopyrimidine compounds 7 (a–b) were synthesized by reaction of 1b and 1,4-dichlorobutane 6 in dimethylformamide under reflux condition. The yields of products following recrystallization were of the order of 60–80%.     

SYNTHESIS OF SOME BICYCLIC OXAZOLO- AND OXAZEPINOPYRIMIDINE DERIVATIVES

Oxazolopyrimidine compounds 2(a–c) and 3(a–e) were synthesized by a simple one-pot condensation reaction of the pyrimidine derivative 1 with 1,2-dibromoethane and 2-bromopropanoic acid, respectively. In a similar way the oxazepinopyrimidine compounds 4(a–b) were synthesized by reaction of 1 and 1,4-dichlorobutane in dioxane under reflux condition. The yields of products following recrystallization were of the order of 55–85%.     

几个新型二茂铁衍生物的合成

二茂铁及其衍生物作为油类消烟剂、燃速催化剂等已得到应用,在药物、合成材料等方面亦具有应用前景。文献曾报道含二茂铁基β-二酮的合成及以它为配体的金属配合物。此类配合物均含两个以上金属原子,它们在有机合成中具有独特的催化活性。 我们将二茂铁甲酰丙酮分别与水扬酰肼、异菸肼、乙二胺及硫代氨基脲在甲醇或甲醇-水介质中进行缩合反应,合成了4个新型二茂铁衍生物,它们含有三个或四个配位功能基团,可作为多齿配体用于金属有机配合物的合成。衍生物的合成路线如下:     

一系列新的二元西佛碱钴(Ⅱ)配合物的合成

Ｎ,Ｎ’双(2羟基苯亚甲基)邻苯二亚胺合钴(Ⅱ)具有可逆加合分子氧的性质[1],因此可作为烃类氧化反应的催化剂[2],但有关这类络合催化剂的取代基效应,尤其是二胺芳环上的取代基对其稳定性和催化活性的影响则未见报道。为此,我们设计合成了在不同芳环上含不同电负性取代基的双水杨醛缩邻苯二胺新配体Ｌ1Ｈ2～Ｌ8Ｈ2及其钴(Ⅱ)配合物ＣｏＬ1～ＣｏＬ8,以期研究其取代基对ＣｏＬ的载氧性能和催化活性的影响。Ｒ1ＨＨＨＨＯＨＯＣＨ3ＯＣＨ3ＯＣＨ3Ｒ2ＨＨＨＨＨＯＣＨ3ＯＣＨ3ＯＣＨ3Ｒ35ＣＨ35ＮＯ23ＮＯ25ＯＣＨ3ＨＨ5ＮＯ24ＯＨＬＬ1Ｌ2Ｌ3Ｌ…     

SYNTHESIS OF SOME DITHIOCARBAMATE DERIVATIVES AND THEIR ANTIMICROBIAL ACTIVITY

Some new, 2-[(N-substituted aminothiocarbonylthio)acetyl]aminothiazole, N-substituted aminothiocarbonylthioacetylaminodiphenylmethane and 9-[(N-substituted aminothiocarbonylthio)acetyl]aminofluorene derivatives were synthesized by reacting 2-(chloroacetyl) aminothiazole, chloroacetylaminodiphenylmethane, and 9-(chloroacetyl)aminofluorene with secondary amine dithiocarbamate derivatives in acetone respectively. The structure elucidation of the compounds was performed by IR, ¹H-NMR, and FAB⁺-MS spectral data. The substances were tested for their antimicrobial activity.     

PREPARATION OF METHYL ESTER DERIVATIVES OF AMINO ACIDS BEARING HYDROLYSABLE N-PROTECTION

ABSTRACT

A convenient method for the esterification of amino acids bearing labile N-substituents is described. Three compounds, 2(a–c), have been synthesised with retention of an N-trifluoroacetamide or an enamine group.     

一些新的芘衍生物的合成及光物理研究

本文合成了一系列新的芘衍生物，用紫外光谱和稳态荧光光谱方法研究了它们的光物理性质。结果表明，取代烷基几乎不影响芘的吸收光谱，而使芘的荧光光谱振动精细结构消失或部分消失；取代甲酰基的芘衍生物的荧光发射强烈依赖于溶剂的性质，极性溶剂中荧光光谱无精细结构，且荧光发射峰随介质极性的增加而红移。     

A FACILE SYNTHESIS OF HETEROCYCLE SUBSTITUTED CHALCONE AND 5-NITROFURANYL OLEFIN DERIVATIVES

Reaction of heterocycle substituted telluronium salts with aroma-tic aldehydes under mild conditions gave corresponding chalcones.In thepresence of dibutyl telluride,2-bromomethyl-5-nitrofuran condensed easilywith aromatic aldehydes in THF to afford corresponding olefin derivativesas one-pot reaction.     

SYNTHESIS AND TRIBOCHEMICAL BEHAVIOUR OF SOME MONOTHIOPHOSPHORIC ACID DERIVATIVES

Abstract

Diisopropylphosphite reacts with sulphur and ammonia to form ammonia monothiophosphoric acid-diisopropylester which, by subsequent reaction with different monochloroacetic acid esters, yields the corresponding monothiophosphoric-acid-O,O-diisopropyl-S-carboalkoximethylesters. These compounds show different wear- and friction-reducing properties in lubricating oils. The tribochemical activity at higher temperatures increases with the chain length of the carboxylic ester group. Auger electron spectroscopy (AES) of the worn metal surface shows that the wear reducing properties correspond with the phosphorus content in the metal surface produced by tribofragmentation of the monothiophosphates. A possible explanation of this effect is discussed.     

SYNTHESIS AND CHEMISTRY OF SOME NEW 2-MERCAPTOIMIDAZOLE DERIVATIVES OF POSSIBLE ANTIMICROBIAL ACTIVITY

4,5-Diaryl-2,3-dihydro-2-mercaptoimidazoles (2a–e) were synthesized. They reacted with chloroacetic acid in gl. acetic acid/Ac ₂ O in presence of anhyd. sodium acetate afforded 5,6-diaryl-2,3-dihydro-imidazo[2,1-b]thiazol-3-ones (3a–d). Also these compounds were prepared by the action of chloroacetyl chloride on compounds (2) in pyridine. Compounds (3a–d) on condensation with aromatic aldehydes yield 2-arylmethylene-5,6-diaryl-2,3-dihydroimidazo[2,1-b]-thiazol-3-ones (4a–q). The latter compounds were prepared directly by the reaction of (2) with chloroacetic acid and the aromatic aldehydes. Compounds (3a–d) coupled with aryldiazonium salts in pyridine to give 2-arylhydrazono-5,6-diaryl-2,3-dihydroimidazo[2,1-b]thiazol-3-ones (5a–r). Also compounds (2) when reacted with 2 or 3-bromopropionic acid afford 2,3-di-hydro-5,6-diaryl-2-methylimidazo[2,1-b]thiazol-3-ones (6a–d) and 2,3-di-hydro-6,7-diaryl imidazo-[2,1-b]-1,3-thiazin-4-ones (7a–d), respectively. Compounds (3, 6, and 7) have been cleaved by aromatic amines to give the corresponding 2-(4′,5′-diaryl-2′,3′-dihydroimidazol-2′-yl)thioacetanilide (8a–f), 2-(2′,3′-dihydro-4′,5′-diaryl imidazol-2′-yl)thiopropionamide (9a–c), and 3-(2′,3′-dihydro-4′,5′-diaryl-imidazol-2′-yl)thiopropionamide (10a–d) respectively. All the prepared compounds show considerable antimicrobial activity against bacteria, yeast, and fungi.     

EASY LARGE-SCALE SYNTHESIS OF STERICALLY ENCUMBERED 2-IODOBIPHENYLS AND SOME DERIVATIVES THEREOF

The convenient one-pot reaction of o-bromofluorobenzene (1) with n-butyl lithium and aryl Grignard reagents followed by quenching with iodine affords substituted 2-iodobiphenyls (4) in yields of 45 to 71%. Lithiation of 4 followed by reaction with Me₂SiCl₂ affords the silanes ArSiMe₂Cl 7.     

某些含二茂铁基的酰氧基茂锆配合物的合成

本文由二氯二茂锆和二氯二(甲基环戊二烯基)锆与二茂铁羧酸钠盐反应合成了六种二茂铁酰氧基茂锆配合物,R_2ZrClY:R=C_5H_5,Y=FcCOO(1),FcCH_2COO(2),FcCOCH_2CH_2COO(3);R=CH_3C_5H_4,Y=FcCOO(4),FcCH_2C0O(5),FcCOCH_2CH_2COO(6)(Fc=二茂铁基)。     

SYNTHESIS OF SOME SULFUR-CONTAINING SPIROINDOLE DERIVATIVES

Abstract

The synthesis of some new sulfur-containing spiroindole derivatives is reported. Fluorinated 3′-aryl-2′-phenylimino-spiro[3H-indole-3,6′[4,5′-pyrazolin][4,3-d]thiazolo]2(1H)-ones were prepared by the reaction of 5-(2-oxo-3-indolinylidene)-3-aryl-2-phenylimino-4-thiazolidinones with hydrazine hydrate. The compounds have been characterized on the basis of elemental and spectral studies.     

SYNTHESIS OF SOME NEW TYPE CHRYSANTHEMIC ESTER

Not only is Cantharidinum considered the active principle of antineoplastic drug in Chinese traditional medicine^[1], but also it and its natrii-cantharidas can be used herbicide and defoliant for legume plants. Seen from the structure of nor-cantharidinamine, it is a five-membered ring glutarimide,which is an active group in pesticide.     

在Lewis酸催化下N-苯乙基甘氨酸衍生物的分子内环化反应研究及苯并-3-氮杂环庚酮-1衍生物的合成

本文报导了不同N-苯乙基甘氨酸衍生物在Lewis酸催化下的分子内环化反应的若干规律,以及苯并-3-氮杂环庚酮-1衍生物的合成.