Synthesis and Crystal Structure of 3-（1-Ethyl-1H-indole-3-carbonyl）aminopropionic Acid

3-(1-Ethyl-1H-indole-3-carbonyl)aminopropionic acid has been synthesized by alkylation of 3-(1H-indole-3-carbonyl)aminopropionic acid methyl ester with bromoethane,follo-wed by saponifying and acidating,in 89.0% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of orthorhombic,space group P212121 with a = 8.9490(12),b = 11.1010(15),c = 13.0475(18) ,V = 1296.2(3) 3,Z = 4,Dc = 1.334 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.095 mm-1,Mr = 260.29 and F(000) = 552.The structure was refined to R = 0.0306 and wR = 0.1445 for 2612 observed reflections with I 2σ(I).In the crystal structure,molecules are linked to each other through hydrogen bonds of N(2)-H(2)···O(1) and O(3)-H(3)···O(1),generating a three-dimensional network.     

Synthesis and Crystal Structure of （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.     

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.     

Synthesis and Crystal Structure of 4-（2-Methylene-1-ethyl-3,3-dimethylindoline-2＇-yl）-6,8-dibromo-1＇-ethyl-3＇,3＇-dimethylspiro-[3,4-dihydro-2H-1-benzopyran-2,2＇-indoline]

The title compound of 4-(2-methylene-1-ethyl-3,3-dimethylindoline-2'-yl)-6,8-dibro-mo-1'-ethyl-3',3'-dimethylspiro[3,4-dihydro-2H-1-benzopyran-2,2'-indoline],C33H36Br2N2O,as a dicondensed spiropyran(DC) has been synthesized by indoline in ethanol with 3,5-dibromo-salicyaldehyde.The compound was characterized by elemental analysis and IR spectra.Meanwhile,the crystal of the compound was obtained and determined by X-ray single-crystal diffraction.Crystal data:monoclinic system,space group P21/n,a=12.9699(15),b=12.5196(13),c=19.327(2),β=106.493(3)°,Mr=636.46,V=3009.1(6) 3,Z=4,F(000)=1304,Dc=1.405 g/cm3,μ=2.722 mm-1,R=0.0554 and wR=0.1176 for 6892 independent reflections(Rint=0.0354) and 5699 observed reflections(Ⅰ 2σ(Ⅰ)).     

Synthesis and Crystal Structure of （Z）-5-fluoro-3- （phenyl（（5-（pyridin-3-ylmethyl）thiophen-2- yl）amino）methylene） Indolin-2-one

The crystal structure of the title compound （Z）-5-fluoro-3-（phenyl（（5-（pyridin-3- ylmethyl）thiophen-2-yl）amino）methylene） indolin-2-one （C25H18FN3OS, Mr = 427.50） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P212121 with a = 5.931（1）, b = 12.413（1）, c = 28.102（2） A, V= 2090.4（3） A3, Z = 4, Dc = 1.358 g/cm3, F（000） = 888, μ= 0.186 mm-1, MoKa radiation （2 = 0.71073）, R = 0.041 and wR = 0.105 for 4567 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the indole and thiophene rings are not coplanar with a dihedral angle of 46.26（5）°. Intramolecular and intermolecular N-H＇..O hydrogen bonds together with C-H...π interations can be observed in the lattice.     

Synthesis and Crystal Structure of （ 1S）- 1,1＇-Bis{[N-ethyl-N-（1-methylethyl）-amino ]- carbonyl }-2-（hydroxydiphenylmethyl）-ferrocene

The title complex, （1S）-1,1＇-bis{[N-ethyl-N-（1-methylethyl）-amino]carbonyl}-2- （hydroxyldiphenylmethyl）-ferrocene （[Fe（C24H22NO2）（C11H16NO）]2·H2O, Mr = 1207.13）, was synthesized via （-）-Sparteine-mediated enantioselective directed ortho-lithiation of 1,1‘-bis{[N- ethyl-N-（1-methylethyl）-amino]carbonyl}-2-（hydroxydiphenylmethyl）-ferrocene. The structure of the rifle compound was determined by X-ray single-crystal diffraction. The crystal belongs to the orthorhombic system, space group P212121, with a = 10.266（2）, b = 17.676（4）, c = 34.097（7）A, V = 6187（2）A3, Z = 4, C70H86Fe2N4O7, Dc = 1.296 g/cm^3,μ = 0.527 mm^-1, T= 113（2） K, F（000） = 2568, the final R = 0.0469 and wR = 0.0984 for 13940 observed reflections with I 〉 2σ（I）. The neighboring ferrocene derivatives are joined into dimers via O-H…O=C intermolecular hydrogen bonding by a water molecule. Besides, the dimers form neat rows along the a axis.     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis-（2-（2,3-difluorophenyl）-ethyl）-1,4,7,10-tetraazacyclododecane

The new compound 1,4,7,10-tetrakis-(2-(2,3-difluorophenyl) ethyl) -1,4,7,10-tetra-zacyclododecane 2 has been synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into diamond crystals grown from CH3CN by slow diffusion at room temperature. It crystallizes in the triclinic system,space group P1 with a = 9.543(2) ,b = 10.507(3) ,c = 10.734(3) ,α = 60.979(3) ,β = 81.870(4) ,γ = 84.279(4) o,V = 931.1(4) 3,Z = 1,Dc = 1.307 g/cm3,C40H44F8N4,Mr = 732.79,F(000) = 384,μ = 0.105 mm-1,T = 296(2) K,MoKa radiation(λ = 0.71073) ,R = 0.0494 and wR = 0.0989 for 1589 observed reflections with I > 2σ(I) . Hydrogen bonds and C-H···π stacking interactions in 2 contribute to a supramolecular structure. Moreover,compound 2 has been determined by 1H NMR,13C NMR,MS,IR spectra and elemental analysis.     

Synthesis and Crystal Structure of 10-（3,4-Dichlorophenymethylidyne）-9,10-dihydrofluorene

A novel compound of 10-(3,4-dichlorophenymethylidyne)-9,10-dihydrofluorene (C20H12Cl2, Mr = 323.20) was synthesized via Knoevenagel reaction under microwave irradiation (500 w) within short reaction time (8 min), giving a high yield of product (87%). Its structure was determined by IR, 1H NMR, MS, elemental analysis and X-ray diffraction. The crystal of the new compound is of monoclinic system, space group P21/c with a = 12.8781(13), b = 16.5067(16), c = 7.4656(7), β = 103.567(2)o, V = 1542.7(3)3, Z = 4, Dc = 1.392 g/cm3, μ = 0.413 mm-1, F(000) = 664, R = 0.0569 and wR = 0.1342 for 3355 observed reflections with I > 2σ(I). The crystal structure involves a conjugated system which shows an olefin structure.     

Synthesis and Crystal Structure of 3-（Trichloroacetyl） Indole

1 INTRODUCTION Indole and its derivatives have attracted much at-tention due to their chemical properties as well asbiological activities[1, . They have been widely used 2]as the materials for producing pigment, perfume,plant growth regulators, etc. Recently, it has alsobeen found that some indole derivatives present anti-tumor and antiviral activities[3～5]. During our sear-ches for bioactive compounds, a series of indole deri-vatives were synthesized, among …     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

Synthesis and Crystal Structure of 4-Bromo-5-ethoxy-3-methyl-5- （naphthalen- 1-yl）- 1-tosyl- 1H-pyrrol-2（5H）- one

The title compound 4-bromo-5-ethoxy-3-methyl-5-(naphthalen-1-yl)-1-tosyl-1H- pyrrol-2(5H)-one 1 (C24H22BrNO4S, Mr = 500.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 8.8562(15), b = 18.118(3), c = 14.055(2) , β = 99.855(3)o, V = 2221.9(6) 3, Z = 4, Dc = 1.496 g/cm3, μ = 1.975 mm-1, λ = 0.71073 , F(000) = 1024, R = 0.0607 and wR = 0.1371.     

Synthesis and Crystal Structure of Methyl 12-Bromo- 13,14-furoxan-deisopropyldehydroabietate

1 INTRODUCTION Pine resin is a very abundant renewable natural source mainly composed of diterpenic resin acids with the general formula C19H29COOH, which has been widely applied in industrial manufactures and fine chemicals[1]. Recently, a series of research re- sults show that the resin acid derivatives are poten- tially useful intermediates in the synthesis of drugs active against viruses[2～5]. Their antiviral activity and function as nucleoside analogues or non- nucleoside inhibito…     

N-(1-甲基-4,5-二溴-2-三氯乙酰基)甘氨酸甲酯的合成与晶体结构

合成了N-(1-甲基-4,5-二溴-2-三氯乙酰基)甘氨酸甲酯(C9H10Br2N2O3, Mr=354.01),X-射线单晶衍射确定其属于正交晶系,P2(1)2(1)2(1) 空间群, a=6.4237(18)(A), b=13.445(4)(A), c=14.054(4)(A), α=β=γ= 90°, V=1213.8(6)(A)3, Z=4, Dc=1.937 Mg·m3, μ=6.672 mm-1, F(000)=688.有2257个可观察点[I>2σ(I)],最终R1=0.0275, wR2=0.0682.X-射线晶体结构的分析表明该化合物含羰基、酰胺基、酯基与溴原子,并且通过N(2)H与O(2)分子间氢键连成一维链状结构.     

(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。     

Synthesis,Crystal Structure and Anticancer Property of （Z）-N-（4-Bromo-5-ethoxy-3,5-dimethyl-furan-2（5H）-ylidene）-4-methylbenzenesulfonamide

The novel title compound(Z)-N-(4-bromo-5-ethoxy-3,5-dimethylfuran-2(5H)-yli-dene)-4-methylbenzenesulfonamide 1(C15H18BrNO4S) has been unexpectedly synthesized by the aminohalogenation reaction of ethyl 2-methylpenta-2,3-dienoate with TsNBr2,and characterized by mp,IR,1H NMR,EIMS,ESIHRMS and single-crystal X-ray diffraction.It crystallizes in mono-clinic,space group P21/c with a = 11.714(5),b = 14.106(5),c = 10.402(4) ,β = 97.298(8)°,V = 1704.9(12) 3,Mr = 388.27,Z = 4,Dc = 1.513 g/cm3,μ(MoKα) = 2.549 mm-1,F(000) = 792,the final R = 0.033 and wR = 0.062 for 3098 observed reflections(Ⅰ 2σ(Ⅰ)).     

(2S,4S)-苯甲基-2-(6-氟-1H-吲哚-3-羰基)-4-羟基-吡咯烷-1-羧酸酯的合成

以4-羟基-L-脯氨酸为原料,经Cbz保护、偶联、Mitsunobu反应和水解合成了抗肿瘤新药Birinapant的重要中间体--(2S,4S)-苯甲基-2-(6-氟-1H-吲哚-3-羰基)-4-羟基吡咯烷-1-羧酸酯,总收率83%,其结构经¹H NMR和ESI-MS确证。     

Synthesis and Crystal Structure of Tris(N-p- methylphenyl-3-hydroxy- 2-ethyl-4-pyridinonato)iron(III)

1 INTRODUCTION A number of hydroxypyrones and hydroxypyridinones are being assessed or considered as orally effective chelators for treatment iron or aluminum overload[1,2]. Almost all present and potential applications involve the tris-ligand complexes of metal(III) cations, as for example in administration of iron(III) complexes for the treatment of anaemia[3], and the appropriate isotopes (e.g. 67Ga, 111In, 90Y) for radiotherapy or the isotopes of gadolinium for magnetic resonance …     

Synthesis and Crystal Structure of (Z)-Ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate

The compound (Z)-ethyl 5-(phenylamino)-3-(phenylimino)-3H-1,2-dithiole-4-carboxylate 3 has been synthesized by the reaction of ethylacetoacetate 1 and phenylisothiocyanate 2. Its structure has been established by ¹H NMR, ¹³C NMR, infrared, mass spectra, and x-ray crystallography.