手性5-(R)-(1′R,2′S,5′R)-孟氧基丁内酯并[3,4-b]-2(S)-6(R)-1-N-环己基氮杂环丙烷的合成及晶体结构

环己胺与手性元5-(R)-(1′R,2′S,5′R)-孟氧基-3-溴-2(5H)-呋喃酮的不对称M ichael加成/分子内亲核取代反应,得到含有两个新手性中心的氮杂环丙烷/稠合丁内酯标题化合物。对其进行了谱学表征和X-射线单晶衍射测定。标题化合物分子式为C20H33NO3,M r=335.47,三斜晶系,P1空间群,晶胞参数:a=5.438(11)。A,b=8.117(2)。A,c=11.572(2)。A,α=96.84(3)°,β=94.48(3)°,γ=101.86(3),°V=493.5(2)。A3,Z=1,D c=1.129g/cm3,R=0.0867,wR=0.2344。     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Synthesis and Crystal Structure of (p-{2-[p-(5''''-Phenyl-1'''',3'''',4''''-oxadiazole-2''''-yl)-phenyl]- vinyl}-phenyl)-di-p-tolyl-amine

1 INTRODUCTION Triarylamines constitute a well known class of hole conducting material[1～4]. On the other hand , oxadiazole-based compounds as good electron- transporting materials[5,6] have played an important role in the fabrication of multiple-layer light- emitting diode devices. It is well known that, to achieve good performance in electroluminescence (EL) devices, the injection of electron and hole should be in balance[7]. The requirement might be met in a new compound containing …     

Synthesis and Crystal Structure of (E)-[1-Ferrocenyl-2-(4-Chlorophenyl) ethylene]

1INTRoDUCTIoNCurrently,thereisaconsiderableinterestintheinvestigationoforganicandorganometallicmaterialsshowinglargenonlinearopticalresponse.Theirpotentialusehasbeenresearchedindeviceapplicationswhicharerelatedtothetelecommuni-cations,opticalcomputingandopticalinformationprocessing"2i.Onamicroscopiclevel,oneofthemajorphysicalparameterstodecidethenonlinearopticalpropertiesofmaterialsisthemolecularhyperpolarizability,avaluedeterminedbyelectronicandgeometricstructureofmolecule.Thetitlecompoun…     

(1R,2S,5R,8S,9R,10S)-8-甲基-4-氮杂-5-苯基-7-氧杂四环[8.2.1.0~(2,9).0(~4,8)]十三-11-烯-3-酮的合成和晶体结构

为确定内型降冰片烯酰亚胺与甲基格氏试剂反应所得加成产物的结构,合成了标题化合物(C18H19NO2)。其结构通过单晶X-射线衍射分析确定,该晶体属正交晶系,空间群为P212121,a = 6.293(1),b = 14.342(3),c = 16.357(3) 牛琕 = 1476.2(5) ?,Z = 4,Dc = 1.266 g/cm3, (MoKa) = 0.082mm-1,F(000) = 600。晶体结构用直接法解出,最终的偏离因子为R = 0.0535,wR = 0.988。由此晶体结构可确定加成产物为标题化合物,并由1H-NMR数据推测另一加成产物的结构。     

Synthesis and Crystal Structure of 1-[4-(Pyrimidin-2-yl)piperazin-1-ylmethyl]-1H-benzotriazole

1 INTRODUCTION Based on the reported 1.65 ? high resolution crystal structure of spinach KARI (ketol-acid reduc- toisomerase) complex[1], we obtained 279 molecules with low binding energy toward KARI from MDL/ ACD 3D database searching, using program DOCK 4.0[2]. These potential structures provide further information for the design of new KARI inhibitors, one of novel derivatives of which as the title com- pound has been synthesized. Its crystal structure will provide us more inf…     

簇合物[Et4N]2[Mo2S4(SCH2CH2S)2]的合成及晶体结构

以(NH4)2MoS4,Et4NBr,HSCH2CH2SH为原料合成了新的簇合物——[Et4N]2[Mo2S4(SCH2CH2S)2],其结构经X射线四圆衍射仪,IR。UV及元素分析确证。其晶体属单斜晶系。晶胞参数为：a=1．0304(8)nm,b=1．4158(8)sin。c=1．1417(1)nm,V=1．63801nm^3,z=4。晶体结构经块状矩阵最小二乘法修正后,最终偏离因子R=0．084。     

3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯的合成及其晶体结构

以香草醛为原料,经Williamsom反应和Knoevenagel-Doebner反应制得新化合物3-(3-甲氧基-4-羧甲氧基苯基)丙烯酸(2);2与乙醇经酯化反应合成了阿魏酸衍生物——3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯(3),其结构经1H NMR,IR,元素分析和X-射线单晶衍射确证。3属三斜晶系,空间群P-1,晶胞参数a=8.301,b=8.474,c=11.445,α=82.94°,β=86.86°,γ=84.52°,V=794.63,Z=2,Dc=1.289 g·cm-3,R1=0.046 7,wR2=0.101 8。3通过分子间氢键(C-H┈O)形成了二维网状结构。     

螺[1-溴-4-(1R,2S,5R)-l-孟氧基-5-氧杂-6-氧代双环[3.1.0]己烷-2,2'-(3'-α-膦酸二乙酯基-(S)-苯甲氧基-4'-l-(1R,2S,5R)-孟氧基丁内酯)]的晶体结构

报道了标题化合物合成和晶体结构。X-射线结构分析表明,该化合物的分子式为C39H58BrO10P,Mr = 797.74,晶体属于单斜晶系,空间群为P21,晶胞参数a = 12.858(3), b = 25.130(5), c = 14.125(3) ? = 105.15(3), V = 4405(2) ?, Z = 4, Dc = 1.203 g/cm3, ?= 1.019 mm-1, F(000) = 1688,R = 0.0726, wR = 0.1201,共收集到9691个独立衍射点,其中可观测点5638个(I≥2s(I))。每个分子中有6个环,13个手性中心,2个五员环呈信封式构象,并分别与三员环组合成[2.4]螺环和[3.1.0]桥环化合物,4个新生成的手性中心的绝对构型为C(6)(S), C(7)(S), C(3)(R), C(2)(R),新引入的磷酸酯官能团C(9)为S构型。     

Synthesis and Crystal Structure of Spiro[1-bromo(S)-4-(R)-hydroxy- 5-oxa-6-oxo-bicyclo[3.1.0]hexane-2,2''-(3''-diethyl-(-(S)-4''-Cl-benzyloxyphosphonyl-4''-(1R,2S,5R)-menthyloxybutyrolactone)]

The title compound, spiro[1-bromo(S)-4-(R)-hydroxy-5-oxa-6-oxo-bicyclo[3.1.0]-hxane-2,2'-(3'-diethyl-α-(S)-4'-Cl-benzyloxyphosphonyl-4'-(1R,2S,5R)-menthyloxybutyrolactone)] has been synthesized via the tandem asymmetric reaction and it crystallizes in a monoclinic system, space group P21 with a = 11.067(3), b = 12.484(2), c = 12.356(2)(A), β = 101.95°,C29H39BrC1O10P, Mr = 693.93, V= 1670.2(6) (A)3, Z= 2, Dc= 1.380 g/cm3, λ(MoKα) = 0.071073nm, μ = 1.410 mm-1, F(000) = 720, the final R = 0.0570 and wR = 0.0758 for 6190 observed reflections with I ＞ 2σ(I). The structure is characterized by the special combination of biologic phosphonyl group and one cyclopropane as well as two butyrolactones. The intermolecular hydrogen bond between O(3)-H(3A)…O(10) in the crystal lattice has been observed.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis,Crystal Structure and Anticoagulant Activity of 5-Chloro-N-[[（5S）-2-oxo-3-[4-（2- oxopyridin-1 （2H）-yl）phenyl] oxazolidin-5- yl] methyl] thiophene-2-carboxamide①

The title compound(zifaxaban 2, C20H16ClN3O4 S, Mr = 429.87) was synthesized and its crystal structure was determined by single-crystal X-ray diffraction. Zifaxaban crystallizes in monoclinic, space group P21 with a = 5.7900(12), b = 13.086(3), c = 12.889(3) A, β = 100.86(3)°, V = 959.1(3) A3, Z = 2, Dc = 1.489 g/cm3, F(000) = 444, μ = 0.342 mm-1, the final R = 0.0320 and wR = 0.0640 for 2717 observed reflections(I 2σ(I)). The absolute configuration of the stereogenic center in the title compound was confirmed to be S by single-crystal X-ray diffraction. Four existing intermolecular hydrogen bonds help to stabilize the lattice and the molecule in the lattice to adopt an L-shape conformation. Zifaxaban was slightly more active than rivaroxaban 1 in in vitro assay against human FXa and therefore is promising as a drug candidate.     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.     

Synthesis and Crystal Structure of N-(1,3,4-Thiadiazol-2-yl)-1-[1-(6-chloropyridin-3-yl)methy]-5-methyl-1H-[1,2,3]triazol-4-carboxamide

The crystal structure of the title compound (C12H10ClN7OS,Mr=335.78) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic,space group P1 with a=8.4093(11),b=9.4430(12),c=11.1454(14),α=95.508(2),β=111.366(2),γ=115.259(2)°,V=711.42(16) 3,Z=2,Dc=1.568 g/cm3,F(000)=344,μ(MoKα)=0.428 mm-1,the final R=0.0476 and wR=0.1243 for 2353 observed reflections (I > 2σ(I)). The dihedral angles between the pyridine and triazole,thiazole and triazole,and pyridine and thiazole rings are 69.2(1),9.2(1) and 72.7(1)o,respectively. Intramolecular C(8)-H(8B)…O(1) and N(5)-H(5A)…N(4) as well as intermolecular C(5)-H(5)…S(1),C(3)-H(3)…N(6) and N(5)-H(5A)…N(1) hydrogen bonds together with weak C-H…π hydrogen-bonding and π-π stacking interactions contribute to the stability of the structure. There is also evidence for significant electron delocalization in the triazolyl system.     

Synthesis and Crystal Structure of Cubane—typeMolybdenum Cluster ComplexMo4S4（DTP）4[μ—SOP（OEt）2]2

1 INTRODUCTION Trinuclear molybdenum complexes with Mo3(3-S)(-O)n(-S)3n (n = 0~3) cores have been extensively studied on their diversified reactions towards various organic ligands and many metals. Many derivatives with Mo3S4 core have been rationally synthesized from the cation precursor [Mo3S4(H2O)9]4+ and its neutral derivative Mo3(3-S)(-S)3(DTP)4(H2O)[1]. However, due to their structural lability, complexes with Mo3(3-S)(-O)n(-S)3n (n = 1~3) cores have been reported limitedl…     

Synthesis and Crystal Structure of N-[1-(4-Chlorophenyl)- 1,4-dihydro-4-oxe-6-methylpyridazine-3-carbonyl]- N'-benzoylhydrazine

1 INTRODUCTION Pyridazinone derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activity. It was widely used in pharmaceuticals and agrochemicals[1, 2]. Rohm Haas Company had reported that pyridazinones exhibit useful plant growth regulating effects [3,4]. It was also reported that diacylhydrazines exhibit excellent insecticides [5~7]. In view of these facts, it was contemplated to synthesize compounds con- taining both pyridazinone …     

Synthesis, Crystal Structure and Properties of 2,7-Bis [4-（diphenylamino）phenyl] fluorene

A novel fluorene derivative containing triphenylamine groups, 2,7-bis[4-(diphenylamino)-phenyl]fluorene (C49H36N2 , Mr= 652.80), was synthesized via Suzuki coupling reaction (yield: 19%) and its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.320(4), b = 11.250(6), c = 17.369(6) , α = 88.035(3), β = 86.450(5), γ = 73.524(5)°, V = 1742.8(13) 3 , Z = 2, Dc = 1.244 g/cm 3 , μ(MoKα) = 0.072 mm -1 , F(000) = 688, S = 1.095, the final R = 0.0616 and wR = 0.1878. It presents a linear framework constituted by a linkage of fluorene as a bridge and two triphenylamine groups. Its spectral and electrochemical properties were studied by UV-Vis absorption, fluorescence spectroscopy and cyclic voltammetry (CV). This compound can emit intense blue fluorescence with a peak wavelength of 446 nm and a full width at half maximum (FWHM) of 38 nm under UV excitation at 350 nm in film. The highest occupied molecular orbital (HOMO) energy level, the lowest unoccupied molecular orbital (LUMO) energy level and optical band gap (Eg) of the title compound are -5.46, -2.57 and 2.89 eV, respectively.     

1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的合成及手性晶体结构

对二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成对二甲氨基苯甲醛缩氨基苯硫脲{1-[4-(dimethylamino)ben- zylidene]-4-phenylthiosemicarbazide}, 并从溶液中析出手性晶体. 元素分析、红外光谱、紫外光谱、核磁谱、质谱和X射线衍射测定其组成和结构. 晶体属正交晶系, P2₁2₁2₁空间群, a＝0.77038(14) nm, b＝1.1428(2) nm, c＝1.6726(3) nm, V＝1.4726(5) nm³, Z＝4, D_c＝1.346 g/cm³, F(000)＝632, μ＝0.219 mm^－1, 可观测点精修最终偏离因子: R＝0.0407, wR＝0.1157. 化合物的晶体结构和固态圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.     

2-氨基-3-氰基-4-(4-氟苯基)-4H-苯并[h]苯并吡喃的合成和晶体结构

标题化合物与N,N-二甲基甲酰胺(DMF)形成的1:1混合结晶物C20H23FN2OC3H7NO由对氟苯甲醛、丙二腈、-萘酚在六氢吡啶存在下合成并经DMF与水的混合溶剂重结晶而得, 其结构通过元素分析、IR 和1H NMR对化合物进行了表征,用X-射线单晶衍射法测定了该化合物的晶体结构。结果表明,晶体属于单斜晶系,P21/n空间群,a = 6.365(1), b = 10.620(2), c = 29.122(6) ? b = 92.00(1), V = 1967.3(6) ?, Mr = 389.42, Z = 4, Dc = 1.315 g/cm3, m (MoKa) = 0.092 mm-1, F(000) = 816。晶体结构用直接法解出,经全矩阵最小二乘法修正,最终偏离因子R = 0.047, wR = 0.1053。化合物分子中,原子C(1), C(2), C(3), C(4), C(5) 和O(1)形成1个六员环,该六员环中C(1)C(2)键长为1.346(3) 牛砻魑肆被肺焦瓜蟆?     

Synthesis, Crystal Structure and Antibacterial Activities of 3-[（2-Hydroxy-4-diethylamino-phenyl）methylenehydrazinocarbonyl]-4-hydroxy-6-methyl-2（1H）-pyridinones

1 INTRODUCTION Recently, compounds containing pyrazole, imida- zole, triazole (including benzotriazole), pyridine, tetrazole and indole have attracted much interest because of their fungicidal activity, plant-growth regulating activity and antibacterial activity[1～3]. Schiff bases also constitute a good type of biolo- gically active substructures[4～7]. Studies of pyri- dine Schiff base-type fungicides have been repor- ted[8]. However, some structures of pyridine com- pounds containing h…