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.     

The crystal structure of 1-(4-chlorophenyl)-3-(4-methylbenzoyl)thiourea

1-(4-Chlorophenyl)-3-(4-methylbenzoyl)thiourea was synthesized and characterized by IR,¹H and ¹³C NMR, mass spectroscopy and the elemental analysis. The crystal structure was confirmed from single crystal X-ray diffraction data. It crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=12.038(3), b=6.330(6), c=18.912(5) Å and β=100.32(3)°. There is a strong intramolecular hydrogen bond of the type N?H...O, with distance N1...O1=2.659(3) Å. The structure is composed of dimers related by inversion centers. The dimers are formed by intermolecular interactions of the type N?H...S with N...S separation of 3.440(2) Å. The mass fragmentation pattern has also been discussed.     

Crystal Structure and Spectral Characters of 2-（4-Methylbenzoly）-3-（4-chlrolphenyl） -4-（1,2,4-triazole）-5-anilino-thiopene

1 INTRODUCTION The triazole derivatives were widely studied because they represent the largest group of modern fungicides and extensively used in both human and veterinary therapy and in agriculture[1～3]. For exam- ple, there are commercially available …     

(E)-1-alkyl-4-

(E)-1-Alkyl-4-[2-(alkylsulfonyl)-1-ethenyl]pyridinium salts were synthesized in two steps. These sulfones were stable at pH 7.3 and underwent a nucleophilic vinylic substitution (S(N)V) with mercaptans, including thiouracile, to give the corresponding 4-(thiovinyl)-pyridinium salts. The X-ray diffraction structure of (E)-1-methyl-4-[2-(ethylsulfanyl)-1-ethenyl]pyridinium iodide indicated conjugation of the sulfur with the pyridinium ring. (Z)-1-Methyl-4-[2-(methylsulfanyl)-1-ethenyl]pyridinium iodide, prepared from the corresponding thioether by reaction with methyl iodide in diethyl ether, underwent isomerization to the E isomer in a first-order reaction in deuterated [D6]DMSO with an activation energy of 14 kcalmol(-1). At pH 7, the (E)-1-methyl-4-[2-(methylsulfonyl)-1-ethenyl]pyridinium iodide (19) reacted specifically with thiols. The reaction of this sulfone with glutathione in a TES buffer at pH 7 was a second-order reaction (k = 4,100 M(-1)s(-1) at 30 degrees C) and gave the corresponding substitution product with an intense long wavelength absorption band (lambdamax=360 nm, epsilon = 27,500 M(-1)cm(-1)). The modification of different enzymes of known structure with 19 showed the high selectivity of this reagent towards thiol groups and its usefulness in the quantitative determination of free thiol groups in proteins.     

1-(1-Carboxy-2-R-4-methylcyclohex-4-enyl)carbonyl- and 1-(2-R-4-Methylcyclohex-4-enyl)carbonyl-3,5-dimethyl(diphenyl)pyrazoles

1-(1-Carboxy-2-R-4-methylcyclohex-4-enyl)carbonyl- and 1-(2-R-4-methylcyclohex-4-enyl)carbonyl-3,5-dimethyl(diphenyl)pyrazoles have been obtained from the reaction of monohydrazides of 2-R-methyl-4-cyclohexen-1,1-dicarboxylic acids and hydrazides of 2-R-4-methyl-4-cyclohexen-1-monocarboxylic acids with acetylacetone and dibenzoylmethane. The conditions for the formation of the pyrazoles depend on the nature of the substituents in the hydrazide starting materials and the structure of the 1,3-diketone used.     

Synthesis and Crystal Structure of 3-（ 2- Hydroxybenzly ）-4-（ 4- Hydro xybenzylideneamino ）-（1H） - 1,2,4- Triazole-5-Thione and Its Antibacterial Activities

1 INTRODUCTION 2. 1 Physical measurements Azole derivatives, such as pyrazole, imidazole, All solvent and chemicals were commercial rea- triazole(including benzotriazole), tetrazole and indole, gents and used without further purification. Ele- have extensive biological activities. They have be- mental analyses were performed on a PE 1700 CHN come the central focus of studies for agricultural che- auto elemental analyzer. IR spectra were recorded on micals, medicines, plant growth regul…     

Synthesis and Crystal Structure of 2-(4-Fluoro-2-(4-fluorophenoxy) phenyl)-1-(1H-1,2,4-triazol-l-ylmethyl)-3-methoxy-isopropy Alcohol

The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol-z 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-tdazole with sodium methoxide. It be-longs to orthorhombic, space group P212121, with a=9.7229(19), b=11.516(2), c=16.047(3) A, C18H17F2N3O3, Mr-361.35, V=1796.7(6) A3, Z=4, Dc=1.3359 g/cm3, F(000)=752,μ=0.106 mm-1, the final R=0.0329 and wR=0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis and Crystal Structure of (E)-4-(Benzyloxy)-2-(cinnamoyloxy)-N,N,N-trimethyl-4-oxobutan-1-aminium Chloride as a Double-prodrug

A novel hydrochloride quaternary ammonium salt (E)-4-(benzyloxy)-2-(cinnamo- yloxy)-N,N,N-trimethyl-4-oxobutan-1-aminium chloride (C23H29NO4Cl2, Mr = 454.37) has been synthesized via the sequence of acetylation and esterification by using L-carnitine (L-4-N-trimethy- lammonium-3-hydroxybutyric acid, LC) and cinnamic acid as the starting materials, and its crystal structure was determined by single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P212121 with a = 10.1670(4), b = 10.4488(4), c = 22.9795(11) ?, V = 2441.18(18) ?3, Z = 4, Dc = 1.236 g/cm3, μ(MoKα) = 0.293 mm?1, F(000) = 960, Flack factor = –0.01(11), the final R = 0.0489 and wR = 0.1550 for 3350 observed reflections (I > 2σ(I)) and R = 0.0953 for all 5648 unique reflections. The crystal structure involves a conjugated system which shows a reverse olefin structure.     

Synthesis and Crystal Structure of （4S）-5-（2-Methoxy-2-oxoethylamino）-5-oxo-4-（3,4,5-trimethoxybenzamido） Pentanoic Acid

1 INTRODUCTION Aminopeptidase N (APN), a member of mem- brane-bound zinc-dependent exopeptidase, is known to be high expression on the brush border membran- es of the small intestine and renal proximal tubules[1]. The over-expression of APN has been involved in several pathological conditions including cancer[2], leukemia, diabetic nephropathy[3], rheumatoid arth- ritis[4], angiogenesis[5] and central nervous system di- seases, such as Alzheimer’s disease[6]. This has led to the sear…     

Synthesis and Crystal Structure of 2-（4-Fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H- 1,2,4-triazol-1-ylmethyl）-3-methoxy-isopropy Alcohol

The title compound 2-（4-fluoro-2-（4-fluorophenoxy）phenyl）-1-（1H-1,2,4-triazol- 1-ylmethyl）-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-（4-fluoro- 2-（4-fluorophenoxy）phenyl）-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229（19）, b = 11.516（2）, c = 16.047（3）A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7（6）A^3, Z = 4, Dc = 1.3359 g/cm^3, F（000） = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56（3） and 54.78（2）°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis, Crystal Structure, Antibacterial Activities and Theoretical Computation of 3-（2-Hydroxybenzly）-4-（4-isopropylbenzylideneamino）-（1H）-1,2,4-triazole-5-thione

1INTRODUCTION Recently,compounds containing pyrazole,imida-zole,triazole(including benzotriazole),pyridine,tetrazole and indole have attracted much interest because they exhibit some fungicidal activity,plant-growth regulating activity and antibacterial acti-vity[1～10].Schiff bases also constitute a good type of biologically active substructure[11～14],and the sulfur-containing Schiff bases are particularly effective.Studies of pyrazole Schiff base-type fungicides andtriazole compounds c…     

Synthesis and Crystal Structure of（E）-Ethyl 2-（5-（3-methyl-2-butenyloxy）-2-（3-（4-（3-methyl-2-butenyloxy）phenyl）acryloyl）phenoxy）acetate

The title compound,(E)-ethyl 2-(5-(3-methyl-2-butenyloxy)-2-(3-(4-(3-methyl-2-butenyloxy)phenyl) acryloyl) phenoxy)acetate(1),has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy,ESI-MS,and X-ray single-crystal diffraction.FT-IR,1H-NMR and ESI-MS confirm the functional groups,particularly the ethyl groups in the ester moiety,of the compound.The single-crystal X-ray diffraction has revealed a monoclinic structure,space group P21/n with a = 14.6832(14),b = 7.7581(7),c = 23.075(2),β = 101.670(2)o,V = 2574.2(4) ?3,Z = 4,Dc = 1.235 g/cm,μ = 0.085 mm-1,and F(000) = 1024.The skeleton of chalcone in the molecular structure is coplanar.     

Chiral Auxiliary-Bearing Isocyanides as Synthons: Synthesis of Strongly Fluorescent (+)-5-(3,4-Dimethoxyphenyl)-4-[[N- [(4S)-2-oxo-4-(phenylmethyl)-2-oxazolidinyl]]carbonyl]oxazole and Its Enantiomer

Both (4S-(+)-3-(isocyanoacetyl)-4-(phenylmethyl)-2-oxazolidinone (R)-1 and its enantiomer (S)-1 have been synthesized as potentially useful synthons in asymmetric synthesis. Optically active (+)-5-(3,4-dimethoxyphenyl)-4-[[N-[(4S)-2-oxo-4-(phenylmethyl)-2-oxazolidinyl]]carbonyl] oxazole (S)-2 and its enantiomer (R)-2 obtained by treating 3,4-dimethoxybenzoyl chloride with (S)-1 and (R)-1, respectively, in the presence of the nonionic superbase P(MeNCH(2)CH(2))(3)N, have high fluorescence quantum yields. The molecular structure of (S)-2 obtained by X-ray means is also presented.     

Synthesis, Crystal Structure and Fluorescent Properties of 1-（4-（Dimethylamino）benzylidene）- 4-（naphthalen- 1-yl） Thiosemicarbazide

1 INTRODUCTION Recently, for the fluorescent properties, Schiff base has been more and more important and widely studied in density optical memories, nonlinear op- tics (NLO), organic light-emitting diodes (OLED), polymer LED and electrogenerated chemilumines- cence (ECL)[1~5]. Thiosemicarbazones are a kind of Schiff bases with thiourea and good ligands easily chelating with transition metal ions. Although they have been studied extensively for a long time due to their chemical and b…     

（E）-1-[4-（2-hydroxy-5-methoxybenzylideneamino）-phenyl]ethanone and （E）-1-[4-（2-hydroxy-4-methoxybenzylideneamino） phenyl]ethanone：X-ray and DFT-calculated structures

The isomeric structures of(E)-1-[4-(2-hydroxy-5-methoxybenzylideneamino)-phenyl] ethanone(I) and(E)-1-[4-(2-hydroxy-4-methoxybenzylideneamino) phenyl]ethanone(Ⅱ) ,both C16H15NO3,have been determined using X-ray diffraction techniques and characterized by IR,and their molecular structures have also been optimized at the B3LYP/6-31G(d,p) level using density functional theory(DFT) . The energetic behaviors of the title compounds in solvent media have been examined using B3LYP method with the 6-31G(d,p) basis set by applying the polarizable continuum model(PCM) . The total energies of the title compounds decrease with the increasing polarity of the solvent. In addition,DFT calculations of the title compounds' molecular electrostatic potentials(MEP) were performed at the B3LYP/6-31G(d,p) level of theory. X-ray study shows that the title compounds both have strong intramolecular O-H…N hydrogen bonds. The molecules of Ⅰ are linked into a one-dimensional framework structure by C-H…π interactions,while in Ⅱ,intermolecular π···π interactions result in the formation of infinite chains running along the [010].     

Synthesis,Crystal Structure and Herbicidal Activity of N-（4-Methylbenzyl）-4-（3-fluorophenyl）-4-piperidinol Hydrochloride

A novel compound N-（4-methylbenzyl）-4-（3-fluorophenyl）-4-piperidinol hydrochloride has been synthesized and its structure （C19H23ClFNO, Mr = 335.83） was characterized by elemental analysis, IR, ^1H NMR, MS and single-crystal X-ray diffraction analyses. The crystal belongs to the triclinic system, space group P1 with a = 7.2163（6）, b = 10.7905（9）, c = 12.2651（10） A, α = 109.576（2）,β = 98.407（2）,γ= 95.956（2）°, V= 878.14（13）A3, Z = 2, Dc = 1.270 g/cm^3,μ = 0.231 mm^-1, F（000） = 356, S = 1.100, the final R = 0.0525 and wR = 0.1425 for 3206 unique reflections （Rint = 0.0140） with 2736 observed ones （I 〉 2σ（I））. The piperidine ring exhibits a chair conformation. The dihedral angle made by the methyl- and fluoro-substituted benzene rings is 66.84（7）°. There are some intra- and intermolecular hydrogen bonding interactions among the molecules, which stabilize the whole crystal structure. The preliminary biological activity tests indicate good herbicidal activity for the title compound, in particular against the roots of some tested plants （such as Brassica campestris L. and Echinochloa crusgallis L.）.     

Synthesis and Crystal Structure of (Z)-Ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1-, with a = 8.140(3), b = 11.966(4), c = 13.771(5) α = 67.366(4), β = 85.165(5), γ = 75.806(4)°, V = 1200.1(7) 3, Z = 2, C26H30O8, Mr = 470.50, Dc = 1.302 g/cm3, F(000) = 500, λ(MoKα) = 0.71073 , μ = 0.096 mm–1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I > 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.     

4-(4-溴丁基)苯乙烯的合成

4-(4-溴丁基)苯乙烯的合成;溴丁基苯乙烯;对氯苯乙酮;对氯苯乙烯;合成     

噻吩甲酰三氟丙酮合铕螯合物(TTA)_4Eu(4—MePy)H的分子结构

题目所指化合物分子式为(C_8H_4O_2F_3S)_4·Eu·(C_6H_7N)H,分子量1130.4,晶体空间群PT,晶胞参数a=16.323;b=12.364;c=11.714;α=108.54,β=90.22,Υ=102.36°;晶胞中有两个分子。由重原子法解出铕原子的位置,用加权傅里叶综合解得粗结构。经块对角矩阵最小二乘修正,偏离因子R=0.046。     

Synthesis,Crystal, Computational Study and Biological Activity of N-(1-(2,4-Dichlorophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl)-4-(N,N-dipropylsulfamoyl)benzamide

The title compound N-(1-(2,4-dichlorophenyl)-1 H-pyrazolo[3,4-d]pyrimidin-4-yl)-4-(N,N-dipropylsulfamoyl)benzamide was synthesized by the condensation of 4-(dipropylsulfamoyl)benzoic acid with 1-(2,4-dichlorophenyl)-1 H-pyrazolo[3,4-d]pyrimidin-4-amine. This intermediate was prepared from 5-amino-1-(2,4-dichlorophenyl)-1 H-pyrazole-4-carbonitrile by the condensation with triethyl orthoformate and then cyclisation with ammonium hydroxide solution in tetrahydrofuran at room temperature. The crystal structure of the title compound was determined. The optimized geometric bond lengths and bond angles obtained by using density functional theory(DFT) have been compared with X-ray diffraction values. In addition, the preliminary biological test showed that the compound possesses distinct effective inhibition on the proliferation of some cancer cell lines.