Synthesis,Structure and Fluorescence Study of 3-Bromo-7-methyloxy-4-methylcoumarin

Coumarin derivative 3-bromo-7-methyloxy-4-methylcoumarin(C11H9BrO3) was synthesized and characterized by FT-IR,1H NMR spectra,and thermal analysis.The crystal structure was determined by X-ray single-crystal diffraction.The title compound crystallizes in the mono-clinic system,space group P21/n,with a = 7.770(16),b = 12.501(3),c = 10.627(2),β = 98.46(3)°,Mr = 269.09,V = 1021.0(4) 3,Z = 4,Dc = 1.751 g/cm3,μ = 4.008 mm-1,F(000) = 536,R = 0.0650 and wR = 0.1463.The optimization of the title compound was obtained by quantum chemical method at the SVWN5/6-31G** level.In the structure,the measured angles of the crystal structure are similar to those calculated,while the measured bond lengths are shorter than the calculated values due to the crystal field which functions to the molecule.The title compound also shows good fluorescent behaviors and good linear relationship with the equal concentration gradient in methanol.     

Extraction and Crystal Structure of Karounidiol

1 INTRODUCTION Karounidiol is a natural pentacyclic triterpene compound, which was identified as a novel compound initially from the Japanese commercial seeds of Trichosanthes kirilowii Maxim. (Fam. Cucurbitaceae)[1], and then isolated from the Chinese commercial seeds of T. kirilowii Maxim. and T. rosthornii Harms[2, 3] and the Japanese wild plant seeds of T. cucumeroides (Ser.) Maxim.[4]. It has not been isolated from other plants up to now, so we are thinking about how to use th…     

多齿配体2,5-二羟基-1,4-苯醌缩氨基脲 (C_6H_4O_3NNHCONH_2.CHON(CH3_)_2)的合成及晶体结构

报道了含1个溶剂DMF的多齿配体2,5-二羟基-1,4-苯醌缩氨基脲的合成和晶体结构。该化合物(C10N4O5H14)属正交晶系,其空间群为P212121 a=13.221(6),b=17.709(5),c=5.347(4)?, V=1252.0(1)3,Z=4,F(000)=568, Dx=1.434g/cm3,Mr=270.25, m (MoKα)= 1.16 cm-1, 结构由直接法解出,全矩阵最小二乘法修正,最终的偏离因子R=0.0319,wR=0.0748。结构测定表明溶剂DMF分子和2,5-二羟基-1,4苯醌缩氨基脲间形成很强的氢键,后者可看作是两条共轭链的偶合物。     

Synthesis and Crystal Structure of 2,2＇-Dihydroxy-[1,1＇]binaphthalenyl-3,3＇-bis-hydroxamic Acids

The first synthesis and structural characterization by X-ray crystallography of racemic 2,2'-dihydroxy-[1,1']binaphthalenyl-3,3'-bis-hydroxamic acids were reported.The com-pound(C28H30N4O8,Mr = 550.56) crystallizes in orthorhombic system,Fdd2 space group with a = 13.055(3),b = 34.871(7),c = 12.570(3) ,V = 5722(2) 3,Z = 8,Dc = 1.278 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.095 mm-1,F(000) = 2320,S = 1.021,R = 0.0349 and wR = 0.0802 for 1757 observed reflections with I > 2σ(I).The N-H and O atom are involved in two-dimensional intermolecular hydrogen bond nets,which further stabilize the structure.     

大环多胺配体BDBPH的设计合成及其晶体结构

用Pb(SN)₂作模板,2,6-二甲酰基对甲苯酚与二亚乙基三胺通过[2+2]缩合反应,经NaBH₄还原、脱Pb²⁺、酸化等操作,得晶体BDBPH·6HBr·4H₂O.晶体属单斜晶系,P2_1/c空间群,晶体学参数:a=1.4441(5)nm,b=1.1482(4)nm,c=1.2090(6)nm,α=90°,β=96.92°,γ=90°,V=1.9900nm³大环分子采取椅式构型,6个Br-和4个H₂O分子对称分布于大环两侧.该大环配体结构新颖,可用于多种金属配合物的研究,对进一步了解金属酶活性中心的结构及其催化作用机理具有重要价值.     

Induced production of novel prenyldepside and coumarins in endophytic fungi Pestalotiopsis acaciae

Concomitant supplementation of a histone deacetylase inhibitor, suberoylanilide hydroxamic acid, and a DNA methyltransferase inhibitor, 5-azacytidine, to the culture medium of a plant endophytic fungus, Pestalotiopsis acaciae, dramatically altered its metabolic profiles. As a result, three novel aromatic compounds, 2′-hydroxy-6′-hydroxymethyl-4′-methylphenyl-2,6-dihydroxy-3-(2-isopentenyl)benzoate (1), 4,6-dihydroxy-7-hydroxymethyl-3-methylcoumarin (2) and 4,6-dihydroxy-3,7-dimethylcoumarin (3), were isolated, along with five known polyketides, endocrocin (4), pestalotiollide B (5), pestalotiopyrone G (6), scirpyrone A (7) and 7-hydroxy-2-(2-hydroxypropyl)-5-methylchromone (8).     

Crystal Structure of 7,3''''-Dihydroxy-4''''-methoxyisoflavone

1 INTRODUCTION Isoflavones and flavones are known to exhibit various biological activities, such as antioxidant[1～3], antiviral[4] and antibacterial[5]. The biological activi- ty of some compounds seems to depend on certain key structure and conformatio…     

无溶剂条件下离子液体催化香豆素衍生物的绿色合成(英文)

Brnsted acidic ionic liquids, namely 2-pyrrolidonium hydrogen sulfate, N-methyl-2-pyrrolidonium hydrogen sulfate, N-methyl-2-pyrrolidonium dihydrogen phosphate, (4-sulfobutyl)tris(4-sulfophenyl)phosphonium hydrogen sulfate, and triphenyl(propyl-3-sulfonyl)phosphonium toluenesulfonate, catalyzed efficient Pechmann condensation of phloroglucinol with β-keto ethyl/ methyl esters. 5,7-Dihydroxy-4-methylcoumarin and 5,7-dihydroxy-4-phenylcoumarin were prepared in good to excellent yields under mild, ambient, and solvent-free conditions. Pyrano[2,3-h] coumarins were then prepared by one-pot three-component reactions of 5,7-dihydroxy-4-subsituted coumarin, malononitrile, and aldehydes in the presence of catalytic amounts of Br nsted basic ionic liquids, namely 2-hydroxyethylammonium formate, 3-hydroxypropanaminium acetate, 1-butyl-3-methylimidazolium hydroxide, pyrrolidinium formate, and pyrrolidinium acetate, under thermal solvent-free conditions. The catalysts are environmentally benign and can be easily prepared, stored, and recovered without significant loss of activity.     

Nitrosodicyanmethanid-Komplexe von Palladium(II) und Platin(II)

Crystal and Molecular Structure of 1,8-Dihydroxy-3,6-dithiaoctan-bis-mercury(II) Chloride The crystal structure of 1,8-dihydroxy-3,6-dithiaoctane-bis-mercury(II) chloride has been determined by X-ray crystal structure analysis. The compound crystallizes monoclinic, space group C2/c with a = 15.311(2), b = 5.870(2), c = 17.479(2) Å, β = 102.76° and 4 formula units per unit cell. The structure was solved by heavy atom technique and refined to a final R value of R = 0.050. Mercury is digonally coordinated by an S and a Cl ligator. In consequence of weak interactions to an oxygen atom of the ligand as well as to three further Cl ions the coordination number is increased to six and a strongly distorted octahedron is formed. The crystal structure is built up from polymeric complex molecules.     

主体分子2,2′-二羟基-1,1′-二萘与客体分子乙酸乙酯晶态包结物的研究

用X射线单晶衍射分析法研究主体分子2，2’-二羟基-1，l’-二萘与客体分子乙酸乙酯（3：1）晶态包结物的晶体结构。其化学式为C64H50O8，Mr=947．08。晶体属三斜晶系，空间群为P1。晶胞参数：个独立衍射点，5823个可观察点（F≥3σF）。2，2’-二羟基-1，1’-二萘与乙酸乙酯形成以氢键联系的包结物3个主体分子中的6个羟基形成21环的氢键体系。     

杯［4］芳烃衍生物一维超分子的晶体结构研究

杯芳烃是继冠醚、环糊精之后的第三代主体分子 ,在主客体化学、超分子化学中占有重要地位 [1～ 3] .据文献报道 ,在杯 [4]芳烃衍生物中存在各种各样的作用力 [4 ] ,如分子内氢键 [3,4 ]、分子间氢键 [5]、阳离子 -π作用 [6 ]、CH3-π作用 [7]和 π-π相互作用 [8,9]等 .本文报道了杯 [4]芳烃衍生物 5 ,1 1 ,1 7,2 3 -四叔丁基 -2 6,2 8-二 [2 -(甲氧基羰基 )苄氧基 ]-2 5 ,2 7-二羟基杯 [4]芳烃 (简称 L,结构式见 Scheme1 )的晶体结构 .研究中发现 ,分子中存在分子内氢键和分子间π-π相互作用 ,后者使化合物 L形成了一维锯齿形的超分子…     

Five new peltogynoids from underground parts of Iris bungei: a Mongolian medicinal plant

Five new peltogynoids, irisoids A-E (1-5), have been isolated from the underground parts of Iris bungei. The structures of the new compounds were established on the basis of spectroscopic methods and were found to be 1,8,10-trihydroxy-9-methoxy-[1]benzopyrano-[3,2-c][2]-benzopyran-7(5H)-one (1), 1,8-dihydroxy-9,10-dimethoxy-[1]benzopyrano-[3,2-c][2]-benzopyran-7(5H)-one (2), 1,10-dihydroxy-8,9-dimethoxy-[1]benzopyrano-13,2-c][2]-benzopyran-7(5H)-one (3), 1,8-dihydroxy-9,10-methylenedioxy-[1]benzopyrano-[3,2-c][2]-benzopyran-7(5H)-one (4), and 1,8,11-trihydroxy-9,10-methylenedioxy-[1]benzopyrano-[3,2-c][2]-benzopyran-7(5H)-one (5). The structure of irisoid B (2) was established unambiguously by X-ray diffraction study.     

Hydrothermal Synthesis and Crystal Structure of a Cd~(2+) Supramolecular Coordination Complex{[Cd_2(HCAM)_2(H_2O)_4]·3.5H_2O}_n with a 3D Metal-organic Open Framework

<正>A three-dimensional coordination polymer {[Cd_2(HCAM)_2(H_2O)_4]·3.5H_2O}_n was synthesized by the hydrothermal reaction of H_3CAM(H_3CAM=4-hydroxypyridine-2,6-dicerboxylic acid)and Cd(NO_3)_2·4H_2O.The structure was characterized by elemental analysis,thermal gravimetric analysis,infrared spectroscopy and single-crystal X-ray diffraction.It crystallizes in triclinic,space group P_1~-with a= 9.4389(19),b=11.009(2),c=11.192(2)(?),α=87.87(3),β= 74.63(3),γ=81.22(3)°,V=1108.2(4)(?)~3,Z=2,D_c=2.164g/cm~3,μ=2.011 mm~(-1),F(000)=710,R =0.0419 and wR=0.1170.X-ray analysis reveals that the title compound adopts a one-dimensional staircase structure by carboxyl of H_3CAM and water molecules,and it is further linked by hydrogen bonds to form a 3-D metal-organic open framework.The thermal gravimetric analysis displays that the framework exists stably below 300℃.     

CS2N3(-)-containing pseudohalide species: an experimental and theoretical study

The first structural reports of anhydrous salts containing the CS2N3 moiety are presented. The new M(+)CS2N3- species (M = NH4 (1), (CH3)4N (2), Cs (3), K (4)) were characterized by vibrational spectroscopy (IR, Raman), as well as multinuclear NMR spectroscopy (1H, 13C, 14N NMR). Moreover, the solid-state structures of NH4CS2N3 (1) [orthorhombic, Pbca, a = 10.6787(1) A, b = 6.8762(1) A, c = 15.2174(2) A, V = 1117.40(2) A3, Z = 8] and (H4C)4NCS2N3 (2) [monoclinic, P2(1)/m, a = 5.9011(1) A, b = 7.3565(2) A, c = 10.9474(3) A, beta = 91.428(1) degrees, V = 475.09(2) A3, Z = 2] were determined using X-ray diffraction techniques. The covalent compound CH3CS2N3 (5) was prepared by the reaction of methyl iodide with sodium azidodithiocarbonate and was characterized by vibrational spectroscopy (IR, Raman), multinuclear NMR spectroscopy (1H, 13C, 14N), and X-ray diffraction techniques [monoclinic, P2(1)/m, a = 5.544(1) A, b = 6.4792(7) A, c = 7.629(1) A, beta = 105.53(2) degrees, V = 264.06(7) A3, Z = 2]. Furthermore, the gas-phase structure of 5 was calculated (MPW1PW91/cc-pVTZ) and found to be in very good agreement with the experimentally determined structure. Improved synthetic routes for the recently reported dipseudohalogen (CS2N3)2 and interpseudohalogen CS2N3CN (6) are described, and the calculated gas-phase structure of 6 was compared with the experimentally determined structure (X-ray). The vibrational spectra of 6 and HCS2N3 (7) are also reported. Furthermore, several plausible isomers for 7 were calculated in an attempt to rationalize the experimentally observed structure which has N-H and not S-H connectivity. The lowest energy isomer for 7 is in agreement with the experimentally observed structure, and the Br?nsted acidity was calculated at the MPW1PW91/cc-pVTZ level of theory. The unknown CSe2N3- anion (8) was also investigated both theoretically and experimentally, and the structure and vibrational data for the unknown CTe2N3- anion (9) were investigated by quantum-chemical calculations using a quasi-relativistic pseudopotential for Te (ECP46MWB) and a cc-pVTZ basis set for C and N. The gas-phase structure of 9 is predicted to be that of a five-membered ring in analogy to the sulfur and selenium analogues.     

Synthesis and Crystal Structure Analysis of 4-Dibenzaldehydeamino-4H-1,2,4-triazole Diacetate

The new title compound 4-dibenzaldehydeamino-4H-1,2,4-triazole diacetate （C16H18N8O4,Mr = 386.38） has been prepared and its crystal structure was determined by single- crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 8.1371（17）,b = 7.1237（12）,c = 16.325 （2）A,β = 100.366（2）°,V = 930.9（3） A^3,Z = 2,Dc = 1.378,F（000） = 404,μ = 0.104 mm^-1,MoKa radiation （λ = 0.71073 ）,R = 0.0307 and wR = 0.1196 for 4632 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule is not flat and the crystal structure is stabilized mainly by van der Waals interactions.     

黑紫橐吾化学成分的分离与鉴定

利用各种色谱技术对黑紫橐吾的乙酸乙酯萃取部位进行分离纯化, 并且根据一维和二维波谱数据进行结构鉴定. 共分离得到4个呋喃雅槛蓝型倍半萜: 1α-氯-6β-异丁酰基-9-酮-10β-羟基-呋喃雅槛蓝烷(1), 1α-羟基-6β-异丁酰基-9-酮-10β-氢-呋喃雅槛蓝烷(2), 1α-羟基-6β-异丁酰基-9-酮-10α-氢-呋喃雅槛蓝烷(3)和1α,10β-二羟基-6β-当归酰基-9-酮-呋喃雅槛蓝烷(4). 其中化合物1为新化合物, 并且通过X射线单晶衍射确定了绝对构型; 化合物2~4为首次从该植物中分离得到.     

Synthesis and Crystal Structure of a Genistein-derived Compound

A genistein derivative, 5-hydroxy-3-（4-hydroxyphenyl）-7-（2-（piperidin- 1-yl）ethoxy）- 4H-chromen-4-one 3, was designed, prepared and structurally characterized by single-crystal X-ray diffraction. X-ray structure analysis reveals that 3 crystallizes in the orthorhombic system, space group Pbca, with a = 16.238（3）, b = 10.308（2）, c = 22.987（5）A, V = 3847.6（13）A3, Z = 8,μ= 0.093 mm^-1, Dc = 1.317 g/cm^3, F（000） = 1616, R = 0.0789 and wR = 0.1554 for 1463 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of 3a-Hydroxy-3-phenyl-1,2,3,3a,8a-pentahydrocyclopenta[α]inden-8-one

The title compound 3a-hydroxy-3-phenyl-1,2,3,3a,8a-pentahydrocyclopenta[α]inden-8-one 2 (C18H16O2, Mr = 264.31) has been obtained by the treatment of 2-(3-iodopropyl)-2phenylindan-1,3-dione 1 with tributyltin hydride in refluxing benzene, and its crystal structure was determined by single-crystal X-ray diffraction. The analysis was carried out by direct and Fourier methods and the structure was refined by full-matrix least-squares computations. The title compound crystallizes in monoclinic, space group P21/n with a = 9.947(3), b = 10.336(3), c = 13.239(4) (A), β = 95.565(6)o, V = 1354.7(7) (A)3, Z = 4, Dc = 1.296 g/cm3, μ(MoKα) = 0.083 mm-1, F(000) = 560, the final R = 0.0749 and wR = 0.1191. X-ray analysis revealed that the bond length of O(2)C(12) is 1.219(2) (A), slightly longer than that of the normal C=O bond (1.119 (A)). The dihedral angle between planes II and III is almost 180°, while plane II is almost vertical to plane I consisting of C(1), C(3), C(4) and C(5) with the deviation of C(2) being 0.6269 (A). In addition, there exist intermolecular hydrogen bonds between O(2) and H(1)-O(1) in the crystal structure.     

The Crystal structure of Hexakisammonium Diacetyloctamolybdate Tetrahydrate

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｓｔｕｄｉｅｓｏｎｏｒｇａｎｉｃｐｏｌｙｏｘｏｍｅｔａｌｌａｔｅｓｈｅｌｐｔｏｕｎｄｅｒｓｔａｎｄｔｈｅｒｏｌｅｓｏｆｐｏｌｙｏｘ ｏｍｅｔａｌｌａｔｅｓｏｎｃａｔａｌｙｓｉｓ.Ａｓｅｒｉｅｓｏｆｏｃｔａｍｏｌｙｂｄａｔｅｓｗｉｔｈｄｅｓｃｒｉｐｔｉｏｎ〔Ｍｏ8Ｏ2 6Ｘ2 〕2ｎ -4(ｎｉｓｔｈｅｎｏｒｍａｌｃｈａｒｇｅｏｆｔｈｅｃｏｏｒｄｉｎａｔｅｄｂａｓｅＸ)ｈａｖｅｂｅｅｎｒｅｐｏｒｔｅｄｉｎｌｉｔｅｒａｔｕｒｅｓ .Ｔｈｅｉｒｓｔｒｕｃｔｕｒｅｓｏｆｔｈｅα ,β ,γ …     

Isolation and Crystal Structure of Horminone

1　INTRODUCTIONhorminoneRabdsia serra( Maxim) hara,a tradi-tional Chinese medicine for the treatmentofhepatitis,enteritis,acute cholecystitis anddysentery,is a perennial herb distributedmainly in central and southeastern parts ofChina〔1〕.In previous reports,four diter-penoids,Rabdoserrin A,Rabdoserrin B,Excisanin A and Kamebakaurin which be-long to ent- kaurene diterpenoids have beenisolated from this source〔2 ,3〕.Horminonewhich has the structure of abietane quinonewas once isolate…