Synthesis and activities of new 4-hydroxy benzoxazolone derivatives

<正>A series of new 4-substituted benzoxazolone derivatives were synthesized according to a convenient method,their anti-inflammatory and analgesic activities in vivo were evaluated.All of them were new compounds,the structures of all the synthesized compounds were confirmed by ~1H NMR,~(13)C NMR,ESI-MS and HR-MS.Most of the compounds exhibited anti-inflammatory activity.     

Preparation of twelve 1-methyl-2-formyl-5-substituted pyrroles and their hydrazones

Preparation of twelve 1-methyl-2-formyl-5-substituted pyrroles (2a-1), with five of them as new compounds, is described. Their derivatives, i.e., 1-methyl-2-formyl-5-substituted pyrrole phenyl hydrazones (3a-1) and 1-methyl-2-formyl-5-substituted pyrrole (4-nitrophenyl) hydrazones (4a-1) are all new compounds. They have also been prepared and further identified.     

Synthesis and biological evaluation of some novel-3-(5-substituted benzimidazol-2-yl)-5-arylisoxazolines

<正>The synthesis of a new series of 3-(5-substituted benzimidazol-2-yl)-5-arylisoxazolines(6a-h) was achieved in excellent yields by the condensation of 1-(1H-benzimidazol-2-yl)-3-(substituted phenyl)prop-2-en-1-ones(5a-h) with hydroxylamine at room temperature.These 1-(1H-benzimidazol-2-yl)-3-(substituted phenyl)prop-2-en-1-ones(5a-h) were obtained by the condensation of 2-acetyl benzimidazoles(4a-d) with different aromatic aldehydes,which in turn were obtained by the oxidation of 2-(α-hydroxy) ethyl benzimidazoles(3a-d) prepared by the reaction of o-phenylenediamines(1a-d) withα-hydroxy propionic acid 2. The synthesized compounds were characterized by their IR,~1H NMR and MS analyses.These compounds were screened for their antibacterial and antifungal activity by standard methods and found some of them active.     

Syntheses and Structure-Odor Relationship of Some γ-Lactones

A lot of norbornene derivatives and lactones are widely used as fragrant components in food or cosmetics. We expected that a series of new compounds with better odor character could be obtained when these two skeleton structures were combined. Thus, a series of endoand exo-5,5-disubstituted-3-oxo-4-oxatricyclo[5,2,1,0~(2,6)]dec-8-enes(Ⅰ) were synthesized.     

STUDIES ON DERIVATIVES OF 2,3-DIHYDRO-4H-1,3,2-BENZOXAZAPHOSPHORINE——SYNTHESIS AND STRUCTURE ANALYSIS OF 2,3-DISUBSTITUTED-2,3-DIHYDRO-4H-1,3,2-BENZOXAZAPHOSPHORIN-4-ONE-(THIONE)-2-SULFIDE(OXIDE)

A series of novel organocyclophosphorus compounds including twenty-three 2, 3-disubsti-tuted-2,3-dihydro-4H-1,3,2-benzoxazaphosphorin-4-one-2-sulfide (compounds Ⅰ) and three 2, 3-disubstituted-2,3,-dihydro-4H-1,3,2-benzoxazaphosphorin-4-thione-2-oxide (compounds Ⅱ) havebeen synthesized. Their structures were determined by IR, UV, HNMR, X-ray diffractionand elemental analysis. Each of compounds Ⅰ showed a strong absorption between 1290-1319em~(-1) in the IR spectrum. Comprehensive studies of the spectral data and experimental re-sults indicated that this strong characteristic absorption is different from that of the P = Olinkage and thus could be considered as a result of the stretching vibration of (unsaturatedC)-N single bond. In the course of synthesis of the compounds, an abnormal productisomers could be made predominantly in yield and be readily isolated from the other byrecrystallizing for several times from appropriate solvent. Data for the melting point, IR,UV and HNMR spectra of three pairs o     

Synthesis of Novel Chiral 7-Amide Substituted-4-androstene-3,17-dione Derivatives

A series of novel 7-amide substituted-4-androstene-3,17-dione derivatives(8αa 8αh or 8βa 8βh) was synthesized from the important intermediates 5 by N-acylation and acidic hydrolysis.Compounds 5α and 5β were obtained through the reaction sequence including acetalization,allylic oxidation,oximation and reduction.The structures of the target compounds were characterized by MS,1H NMR,13C NMR and HRMS spectra and their stereo configurations were identified through DEPT(distortionless enhancement by polarization ...     

Preparation and Characterization of Chromium(Ⅲ)-Containing α-and β-Tungstosilicates

Eight new compounds of α- and β- M2H4[SiW16Cr2(OH2)2O ] .xH2O types, where M = K, Me4N, Et4N or n-Bu4N, and 0+6=6,were synthesized from trivacant heteropoly tungstate α-and β-[SiW9O34]10 precursors, and characterized by elemental analysis, thermal gravimetric analysis, IR, UV-visible spectra, X-ray photoelectron spectroscopy(XPS), polarography, magnetic measurements and X-ray powder diffraction. The IR and UV spectra conJEirm that α-and β-[SlW10Cr2(OH2)2O24]6- isomers possess α-and β-Keg-gin structures. The differences between α-and β-isomers in IR, UV spectra and polarography are discussed.     

Synthesis and anti-HBV activity of novel 5-substituted pyridin-2(1H)-one derivatives

<正>Four novel 5-substituted pyridine-2(1H)-one derivatives were designed and synthesized by using addition-elimination reactions.The structures of these novelly synthesized compounds were verified by ~1H NMR,ESI-MS and single crystal X-ray diffraction.Furthermore,all four compounds(most notably compound 7a) were found to be highly efficient against hepatitis B virus (HBV) in cultured HepG2 2.2.15 cell,making them promising drug candidates for potential bioactive molecule against hepatitis B.     

β-Tosylamino and/3-Hydroxyl Substituted α-Diazocarbonyl Compounds： X-ray Structure and 1,2-Migrations under Photochemical Condition

As a continuation of the investigation on 1,2-migration of metal carbene and free carbene, two X-ray structures of β-substituted α-diazocarbonyl compounds were obtained. The relationship between the structure and 1,2-migratory aptitude was discussed and an exploratory photochemical study of the diazo compounds presented.     

取代吡唑啉衍生物的合成与生物活性

采用α-三唑-β-烷氧基芳酮与肼关环,制备了1,3-二苯基-4-三唑基吡唑啉1a,1-苯基-3-对氯苯基-4-三唑基吡唑啉1b和3-取代苯基-4-三唑基吡唑啉(7),并研究了化合物7的成环优化条件.使用α,β-不饱和酮与肼关环合成了1,3,4,5-多取代吡唑啉衍生物1c-1h,并初步用质谱法确定了该反应产物的结构;同时,以3,5-二取代吡唑啉(6)和7作为中间体合成了1-,3-,4-或5-取代的化合物2a-2l.初步生物活性测定结果表明,所合成的化合物均有一定的杀菌、激素和除草效果.     

Microbial transformation of diosgenin by Syncephalastrum racemosum (Cohn) Schroeter

<正>Microbial transformation of diosgenin(1) by Syncephalastrum racemosum yielded five new polar metabolites,which wereidentified as(25R)-spirost-5-en-3β,7α,9α-triol-12-one(2),(25R)-spirost-5-en-3β,9α,12α-triol-7-one(3),(25R)-spirost-5-en-3β,9α-diol-7,12-dione(4),(25R)-spirost-4-en-9α,12β,14α-triol-3-one(5),and(25S)-spirost-4-en-9α,14α,25β-triol-3-one(6).Compounds 1-6 exhibited moderate cytotoxicity against K562 cells and among them compounds 2,3,and 6 were more potentthan the parent compound 1.     

宽叶秦岭藤根部的化学成分

通过正相和反相硅胶柱层析从宽叶秦岭藤根部乙醇提取物中分离纯化得到19个化合物,经波谱分析并结合化学方法鉴定了其结构,其中4个为新化合物,它们分别是3,5-二羟基二十烷酸羽扇豆醇酯(3),2-羟甲基-5-甲氧基苯基-O-β-D-吡喃葡萄糖甙(11),Δ5-孕甾烯-3β,20(S)-二醇-20-O-β-D-吡喃葡萄糖基(1→6)-β-D-吡喃葡萄糖甙(18,秦岭藤甙C)和Δ5-孕甾烯-3β,20(S)-二醇-3-O-β-D-吡喃葡萄糖基-20-O-β-D-吡喃葡萄糖基(1→6)-β-D-吡喃葡萄糖甙(19,秦岭藤甙D).     

Benzopyranopyridine derivatives 3. Reaction of 1-azaxanthone with grignard reagents

Three different classes of compounds were isolated in the reaction of Grignard reagents with 5-H[1]benzopyrano[2,3-b]pyridin-5-one, commonly called 1-azaxanthone. The formation of (a) 4-substituted 1,4-dihydro-1-azaxanthones (II), (b) 5-substituted-5-hydroxy-1-azaxanthenes (III) or (c) 4,5-disubstituted-1-azaxanthenes (IV) is dependent on the solvent used in the preparation of the Griganrd reagent (i.e. ether or tetrahydrofuran), the steric properties of the reagent and on the temperature. The isolated compounds were characterized by chemical derivatives and/or spectroscopic analyses.     

One-pot Synthesis of α,β-Dehydroamino Derivatives from β,β-Dicyanostyrene with 1,3-Dibromo-5,5-dimethylhydantoin Promoted by Mild Base

The reaction of β,β-dicyanostyrene derivatives(1) with 1,3-dibromo-5,5-dimethylhydantoin(DBDMH) was systematicly studied. The reaction could generate different products when promoted by different mild bases. When the reaction was promoted by NaOAc(100%, molar ratio to compound 1), β,β-dicyanostyrene derivatives could be directly converted into corresponding α,β-dehydroamino derivatives in good to excellent yields in one-pot. When the reaction was promoted by K₃PO₄(80%, molar ratio to compound 1), the corresponding α,β-dehydroamino and double-α,β-dehydroamino compounds were simultaneously obtained and the total conversion of β,β-dicyanostyrene derivatives was up to 90% or higher.     

含硫碳负离子的反应和应用研究(Ⅶ)——4,4-二取代1,7-二官能团化合物的合成

通过α-芳基磺酰基乙酸乙酯与α,β-不饱和酯、腈、酮在温和条件下进行双共轭加成反应一锅法高产率地合成了一系列1,7-二官能团化合物,对它们的结构作了表征,初步讨论了Michael受体、相转移催化剂和溶剂对该双共轭加成反应的影响。     

草玉梅中的化学成分

从草玉梅根部和地上部分甲醇提取物中分离到的8个化合物,其中三萜内酯(7)和三萜皂甙(8)为新化合物.     

新型可溶性酞菁的合成和光致发光及电致发光性质

以3(4)-硝基邻苯二腈和对甲氧基苯酚为原料, 经过两步反应合成了α(β)-四(4-甲氧基苯氧基)酞菁锌, 通过谱学方法和元素分析表征了其结构. 比较研究其溶液和旋涂膜的紫外可见光谱、光致发光光谱和固体薄片的光致发光光谱. 并以其旋涂膜为发光层制备了电致发光器件, 研究其电致发光性质. 结果表明, 固态酞菁材料与其溶液的荧光发射波长相比均向长波方向移动了145 nm以上, 而且都有不同程度的宽展. 在固态下β-位取代酞菁荧光发射波长红移的程度比α-位取代酞菁大. 电致发光光谱的发射波长和其旋涂膜的光致发光光谱的发射波长基本一致, 大约在856和862 nm左右. 在固态下酞菁分子排列紧密, 分子间相互作用增强导致了荧光发射波长的巨大红移.     

Benzimidazole condensed ring systems. 2. New synthesis of substituted 1-oxo-1H,5H-pyrido[1,2-a]benzimidazole-4-carbonitriles and related derivatives

The synthesis of some 3-substituted and 2,3-disubstituted-1-oxo-1H,5H-pyrido[1,2-a]benzimidazole-4-carbo-nitriles 5,6 by fusing 1H-benzimidazole-2-acetonitrile 1 with some β-keto esters 2,4 in the presence of ammonium acetate or with ethyl β-aminocrotonate 3 is described. The tricyclic compounds were converted to their N-5 methyl of N-5 ethyl derivatives 8,9. Vilsmeir-Haack formylation of 3-methyl-1-oxo-1H,5H-pyrido[1,2-a]-benzimidazole-4-carbonitrile 5a afforded its 2-formyl derivative 10. Chlorination of 5 and 6 with phosphorus oxychloride yielded the respective 1-chloropyrido[1,2-a]benzimidazole-4-carbonitriles 11,12 which were utilized to prepare the 1-azido, 1-amino, 1-piperidino and 1-methoxy derivatives of the ring system. Compound 11a exhibited strong in vitro activity against S. aureus. Four compounds were screened against P-388 lymphocytic leukemia in mice but were inactive.