3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮的合成与晶体结构

在THF溶液中合成了标题化合物3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮,并用FT-IR、UV-Vis、1HNMR、13C NMR、MS、元素分析和X-射线衍射等进行了表征。结果表明此化合物属正交晶系,空间群为Pbca,晶胞参数为:a=15.891(16),b=11.126(11),c=19.778(19),α=β=γ=90°,V=3497(6)3,Z=8,Dc=1.306Mg/m3,μ=0.234 mm-1,F(000)=1440。在化合物的分子结构中,两个苯环几乎垂直于呋喃酮平面,且它们与呋喃酮平面的两面角分别为89.38°和88.19°。     

7,7-二甲基-2-对溴苯基-4-苯基-5-氧代-1,4,5,6,7,8-六氢化-6H-喹啉的合成及晶体结构

标题化合物C23H22BrNO是由1-(4-溴苯基)-3-苯基-2-丙烯-1-酮与5,5-二甲基-1, 3-环己二酮在N, N-二甲基甲酰胺(DMF)中在NH4OAc催化下反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于单斜晶系,空间群C2/C, a = 19.678(4),b = 13.571(2),c = 17.311(3) 牛琤 = 118.74(1),Mr = 408.33, V = 4055(1) ?,Dc = 1.338 g/cm3, Z = 8, m (MoKa) = 2.038 mm-1, F(000) = 1680, R = 0.0539,wR = 0.1369。X-衍射分析表明,六元环C(10)C(13)C(16)C(17)采用半椅式构象:原子C(10),C(11),C(12),C(16)和C(17)在同一个平面内,而原子C(13)远离平面为0.3282 牛闷矫嬗?个苯环的夹角分别为41.09, 81.97,2个苯环的夹角为75.87。另外在晶体结构中,存在1个分子间氢键。     

(Z)-2-羟基-3-苯甲酰丙烯酸甲酯的合成及晶体结构

标题化合物C11H10O4的晶体结构用X-射线单晶衍射法测定。晶体属单斜晶系, P21/c空间群, 晶胞参数a = 12.136(1), b = 5.559(1), c = 14.615(2) ? b = 96.758(3), V = 979.1(3) ?, Z = 4, Mr = 206.19, Dc = 1.399 g/cm3, F(000) = 432, m(MoKa) = 0.107 mm-1。晶体结构用直接法解出, 经全矩阵最小二乘法对原子参数进行修正, 最终的偏离因子为R = 0.0453, wR = 0.0990。标题化合物形成了1个大的共轭体系, 含有1个稳定的烯醇结构。结构测定表明还存在着1个分子内氢键的结构, 它使烯醇结构更加稳定。     

2-(4''''-正丙基苯)咪唑并[2,1-α]异喹啉的晶体结构

本文测定了新型抗早孕药物 2-(4'-正丙基苯)咪唑并[2,1-a]异喹啉的晶体结构。该化合物分子式为C20H18N2, Mr = 286.38, 晶体属单斜晶系, 空间群为P21/n, 晶胞参数为a = 7.2177(1), b = 7.8036(2), c = 27.429(1) ? b = 90.976(3), V = 1544.67(8) 3, Z = 4, Dc = 1.231 g/cm3, F(000) = 608.00, m(Mo-Ka) = 0.073 mm-1, R = 0.0560, wR = 0.1440, 获得25986个衍射点,其中独立衍射点3795个。在分子结构中, 苯环(C(1)C(6))与环(N(1), C(1)C(9))以及咪唑环共平面, 该平面与苯环(C(12)C(17)所在平面的夹角为10.014。     

N,N'-二-[5-甲氧基-3-溴-2(5H)-4-呋喃酮基]-1,2-乙二胺的合成及其晶体结构(英文)

通过串联迈克尔加成-消除反应合成了N,N'-二-[5-甲氧基-3-溴-2(5H)-4-呋喃酮基]-1,2-乙二胺,利用IR、UV、1H NMR、13C NMR、MS、元素分析和X射线单晶衍射对其进行表征.X射线单晶衍射结果表明:标题化合物包含两个平面的呋喃酮环和两个手性中心,并通过N(1)-H(1A)…O(1)分子间氢键和Br(1)…O(2)近距离作用形成超分子结构.     

4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯的合成和晶体结构

2-甲砜基-4,6二甲氧基嘧啶和N-(4-丙氧羰基苯基)-2-羟基苄胺在四氢呋喃溶液中反应, 生成标题化合物4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯,并测定了其晶体结构。该化合物分子式为C23H25N3O5,晶体属单斜晶系,空间群为P2/n,晶胞参数为a = 14.8504(8),b = 9.4420(4),c = 16.3129(9) 牛 = 104.881(1)埃琕 = 2210.6(2) 3,Z = 4,Dc = 1.272 g/cm3,F(000) = 896.00,(MoK? = 0.91 cm-1,R = 0.051,wR = 0.118,获得19761衍射数据,其中独立衍射点5004个。经元素分析、IR、MS和HNMR等对化合物的结构进行了表征。在分子结构中,各有3个不同的共轭平面。嘧啶环和苯环(C(7) C(12)),及苯环(C(14) C(19))的夹角分别为99.18 , 164.15埃?个苯环之间的夹角为94.93啊;衔锍世啻焦瓜蟆?     

N,N′-二[3-氯-5S-(l-孟氧基)-2(5H)-4-呋喃酮基]-1,4-丁二胺的合成及晶体结构(英文)

合成了N,N′-二[3-氯-5S-(l-孟氧基)-2(5H)-4-呋喃酮基]-1,4-丁二胺,并通过IR,1H NMR,MS和X射线单晶衍射对其进行了表征.X射线单晶衍射结果表明:标题化合物的不对称结构单元中包含一个平面的呋喃酮环和一个椅式的环己烷环,四个手性中心.标题化合物通过N—H…O分子间氢键作用实现空间堆积.     

4-苯基-2-对甲氧基苯基-1,5-苯并硫氮杂卓-α,α-二甲基-β-内酰胺的合成及晶体结构

合成了标题化合物并测定了其晶体结构。该化合物的化学式为C26H25NO2S, Mr = 415.53。晶体为三斜晶系,P 空间群,晶胞参数为:a = 9.299(3), b = 10.134(3), c = 12.455(4) ? a = 98.457(5), b = 106.143(5), g = 103.843(5), V = 1065.7(6) 3, Z = 2, Dc = 1.295 g/cm3, F(000) = 440, m = 0.175 mm-1, R = 0.0406, wR = 0.1064。晶体结构显示,化合物中七员环呈类椅式构象,b-内酰胺环近似梯形。     

微波辐射下4-(2-氯苯基)-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的合成和晶体结构

标题化合物C14H15ClN2O3是由2-氯苯甲醛、乙酰乙酸乙酯、尿素在TsOH作用下用微波辐射反应得到, 结构通过单晶X-射线衍射法确定, 其晶体属三斜晶系, 空间群P, Mr = 294.73, a = 7.688(1), b = 9.106 (2), c = 11.412(2) ? = 102.963(3), = 105.957(2), g = 102.484(2), V = 714.9(2) ?, Z = 2, Dc = 1.369 g/cm3, = 0.276 mm-1, F(000) = 308, 最终的偏离因子为R = 0.0845, wR = 0.2092。在分子结构中嘧啶环为船式结构, 平面1(苯环)与平面2 ((C(8)C(9) C(10)N(2))之间的两面角为 91.57啊?     

高效的多组分反应构建N-叔丁基-3-(4-甲氧基苯基)-7,7-二甲基-5-氧-1,4,5,6,7,8-六氢化噌啉-4-甲酰胺化合物及其结构表征

标题化合物C22H29N3O3以简单易得的试剂为原料,在乙醇溶剂中,微波辐射下经两步多组分反应合成得到.其结构通过单晶X射线衍射法确定,晶体属三斜晶系,空间群P-1,相对分子质量Mr=383.48,晶胞参数a=1.147 70(12)nm,b=2.065 7(2)nm,c=1.007 80(12)nm,V=2.184 1(4)nm3,Z=4,晶胞密度Dc=1.166 mg/m3,吸收系数μ=0.078mm-1,单胞中电子的数目F(000)=824.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R1=0.070 9,wR2=0.140 5.在晶体结构中新形成的噌啉环为近似于共平面结构,而其中的哒嗪环则为船式构象.     

Crystal Structure of 5-(l-Menthyloxy)-3-Chloro-4-Pyrrolidinyl-2(5H)-Furanone

１ＩＮＴＲＯＤＵＣＴＩＯＮＯｗｉｎｇｔｏｔｈｅｉｒｗｉｄｅｏｃｃｕｒｅｎｃｅｉｎａｖａｒｉｅｔｙｏｆｂｉｏｌｏｇｉｃａｌｙａｃｔｉｖｅｎａｔｕｒａｌｐｒｏｄｕｃｔｓａｎｄｔｈｅｉｒｕｔｉｌｉｔｙａｓｖａｌｕａｂｌｅｓｙｎｔｈｅｔｉｃｉｎｔｅｒｍｅｄｉ...     

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro[2,3-d]pyrimidin-4（3H）-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.     

Synthesis and Crystal Structure of 2-（ 4-Decarboxydehydroabietyl）- 5-p-tolyl-[ 1,3,4 ]-oxadiazole

2-（4-Decarboxydehydroabietyl）-5-p-toyl-[1,3,4]-oxadiazole, C28H34N2O, has been synthesized and characterized by IR, NMR, elemental analysis and single-crystal X-ray diffraction method. The crystal belongs to the orthorhombic system, space group P212121 with a = 6.1351（5）, b = 14.8495（19）, c = 25.9050（2） A, V = 2360.0（4） A3, Z = 4, Mr = 414.57, Dc = 1.167 Mg/m^3, 2 = 0.71073 A,μ（MoKa） = 0.070 mm^-1, F（000） = 896, the final R = 0.0452 and wR = 0.1076 for 1647 observed reflections with I 〉 2σ（I）. There are five rings in the crystal structure of the title compound, but the oxadiazole ring is non-coplanar with the benzene ring D.     

Crystal Structure of 1, 1-Dichloro-la, 3-diphenyl-1, la, 2, 3-tetrahydro-azirino [2, 1-d ] [1, 5]benzothiazepine (C_(22),H_(17)Cl_2NS )

1INTR0DUCTI0NBenzoheteroazepinecompoundsareimportantpharmaceuticalagents"-".Inre-centyears,ithasbeenfoundthatbenzoheter0azepinetricyclicderivatives,especiallythosefusedwithotherfiveorsix-memberedheterocycle,area1soofpotentialphar-maceuticalinterestst4-6j.Hence,muchattentionhasbeenpaidtothesynthesesofthem,suchasl,3-oxazino[3,2-djt1,5jbenzothia/diazepin-l-onet"'J,1,2,4-tria-zolo[4,3-dj[1,5jbenzothia/diazepine"',1,2,4-oxadiazolo[4,5-dj[l,5jbenzothia/diazepine',',andsoon.Meanwhiletheirstructur…     

Synthesis and Crystal Structure of N,N′-Bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine

The title compound,N,N′-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine(C31H48Cl2N2O6,Mr = 615.61),has been synthesized and characterized by IR,1H NMR,MS,elemental analysis and single-crystal X-ray diffraction.The crystal crystallizes in the monoclinic system,space group C2 with a = 16.1091(4),b = 11.1880(3),c = 19.2854(5) ,β = 106.297(2)°,V = 3336.12(15) 3,Z = 4,Dc = 1.226 mg/m3,μ = 0.237 mm-1,F(000) = 1320,the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections(I > 2σ(I)).X-ray analysis reveals that the title compound possesses four rings:two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation,containing eight chiral centers:C2(S),C3(R),C5(R),C10(S),C18(S),C21(R),C22(S) and C25(R).The structure is stabilized by N-H…O hydrogen bonding interaction.     

Synthesis and Crystal Structure of Ethyl 1-（2-bromoethyl）-3-（4-meth-oxyphenyl）-1H-pyrazole-5-carboxylate

The title compound ethyl 1-(2-bromoethyl)-3-(4-methoxyphenyl)-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic(C15H17BrN2O3,Mr = 353.22),space group C21 with a = 24.691(7),b = 6.7678(17),c = 17.884(5) ,β = 97.184(5)o,V = 2965.1(13) 3,Z = 8,Dc = 1.583 g.cm-3,F(000) = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I > 2σ(I).All the carbon atoms in the molecule are nearly coplanar except C(15),with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.     

Crystal Structure of 3-(4'-Methoxyl)-phenyl-5-cyano- 6-methylthio Pyrimidine-2, 4-diones

1 INTRODUCTIONIt has been reported that various heterocyclic compounds containing nitrogen atoms, especially uracils, have biologically interesting properties in medicinal and pesticidal chemistry as fungicides and herbicides [1]. In our recent research, a novel substituted pyrimidione was synthesized in order to look for new inhibitors with Hill inhibitory [2~4].Preliminary bioassay indicates that some of analogs of the title compound have good Hill inhibitory activity [5].In an attempt…     

Synthesis and Crystal Structure of 2-(4''-Methylphenoxy)-5,8,9-trimethyl-3-phenyl Thieno[3'',2'':5,6]pyrido[4,3-d]pyrimidin-4-(3H)-one Hydrochloride

The title compound 2-(4′-methylphenoxy)-5,8,9-trimethyl-3-phenyl thieno[3′,2′:5,6]pyrido[4,3-d]pyrimidin-4(3H)-one hydrochloride (C26H23Cl4N3O2S, Mr = 583.33) has been deter- mined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 14.8442(11), b = 11.5131(8), c = 17.2010(13) (A), β = 113.7250(10)o, V = 2691.3(3) (A)3, Z = 4, Dc = 1.440 g/cm3, S = 1.094, μ = 0.547 mm-1, F(000) = 1200, the final R = 0.0571 and wR = 0.1458. X-ray analysis reveals that the title compound combines with a molecule of dichloromethane by an intramolecular hydrogen bond. The thienopyridine ring is almost coplanar, and the dihedral angle between the thiophene plane and the pyridine plane is 0.6o.     

Synthesis and Crystal Structure of a Co(II) Complex with Schiff Base and Imidazole Ligand

1 INTRODUCTION The chemical behavior of metal complexes with Schiff base ligand has attracted much attention be- cause of their catalytic activity in some industrial[1, 2] and biochemical processes[3~5]. As some metal com- plexes have shown the catalytic activity in some polymerization reactions[2, 6], we are recently inte- rested in polymerizartion of organo-silicon com- pounds catalyzed by Schiff base complexes of tran- sition metals. A series of Schiff base complexes have been prepare…