Synthesis of methyl 4-aryl-2-{[4-(carbamimidoylsulfamoyl)- phenyl]amino}-4-oxobut-2-enoates

Methyl aroylpyruvates reacted with 4-amino-N-carbamimidoylbenzene-1-sulfonamide in acetic acid–ethanol (1: 1) to give methyl 4-aryl-2-{[4-(carbamimidoylsulfamoyl)phenyl]amino}-4-oxobut-2-enoates which were found to exist in solution as mixtures of Z and E isomers.     

Synthesis and Antiviral Activity of 1-{[2-(Phenoxy)ethoxy]methyl}uracil Derivatives

The synthesis of novel 1-{[2-(phenoxy)ethoxy]methyl}uracil derivatives with different substituents in positions and 6 of the pyrimidine ring has been carried out. It has been shown that the alkylation of trimethylsilyl derivatives of uracil with 2-(4-chlorophenoxy)- and 2-(4-methylphenoxy)ethoxymethyl chloride under Hilbert-Johnson reaction conditions gives N₍₁₎-substitution products. It was found that the 1-{ [2-(phenoxy)ethoxy]methyl}uracil derivatives show viral inhibition properties relative to human immunodeficiency type 1 virus in vitro. The most active compounds are 5-bromo-6-methyluracil derivatives which suppress viral reproduction by 50% at 7.2 and 7.8 micromolar concentrations.__________Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 726–731, May, 2005.     

Bis{[diphenyl(piperidinomethyl)silyl]methyl}cadmium and ‐magnesium

The homoleptic and monomeric metal alkyls bis{[di­phenyl(piperidino­methyl)­silyl]­methyl}cadmium, [Cd(C₁₉H₂₄­NSi)₂] or [Cd{CH₂SiPh₂(CH₂NC₅H₁₀)}₂], (I), and bis{[di­phenyl­(piperidino­methyl)­silyl]­methyl}magnesium, [Mg(C₁₉H₂₄NSi)₂] or [Mg{CH₂SiPh₂(CH₂NC₅H₁₀)}₂], (II), (CH₂NC₅H₁₀ is piperidino­methyl) are isostructural, and the mol­ecules exhibit crystallographically imposed C₂ symmetry. The metal centres are located on special positions and, for each structure, half of the mol­ecule is located in the asymmetric unit. The metal centres are intramolecularly coordinated and stabilized by two piperidino­methyl groups (side‐arm donation). The Si—C and M—C bonds (M is Cd or Mg) are shortened compared with the corresponding non‐metallated compounds, indicating stabilization by the diffuse polarizable Si centres (α effect). The C—M—C angle is 140.53 (12)° in (I) and 123.39 (11)° in (II).     

Synthesis of 2-and 5-(1,1-Dimethyl-1,2,5,6-tetrahydropyridinium-3-yl)oxadiazoline Iodides

ＩｎｔｒｏｄｕｃｔｉｏｎＲｅｃｅｎｔｌｙ ,ｔｈｅｉｎｃｒｅａｓｉｎｇｄｅｍａｎｄｆｏｒｅｆｆｅｃｔｉｖｅｔｒｅａｔ ｍｅｎｔｏｆｎｅｕｒｏｄｅｇｅｎｅｒａｔｉｖｅｄｉｓｅａｓｅｓ ,ｐａｒｔｉｃｕｌａｒｌｙＡｌｚｈｅ ｉｍｅｒ’ｓｄｉｓｅａｓｅ (ＡＤ) ,ｉｓｂｅｃｏｍｉｎｇｍｏｒｅａｎｄｍｏｒｅｕｒ ｇｅｎｔ.ＡｍｏｎｇｔｈｅｒｅｓｅａｒｃｈｅｓｉｎｔｈｅｒａｐｅｕｔｉｃｓｆｏｒＡＤ ,ｍａｎｙｍｕｓｃａｒｉｎｉｃｃｏｍｐｕｎｄｓｎｏｔｏｎｌｙａｒｅｂｅｎｅｆｉｃｉａｌｉｎｔｈｅｔｒｅａｔ ｍｅｎｔｏｆＡ…     

Reaction of 2-{[2-(ethenyloxy)ethoxy]methyl}oxirane with oxazolidin-2-ones

Reactions of 2-{[2-(ethenyloxy)ethoxy]methyl}oxirane with N-unsubstituted oxazolidin-2-ones give mixtures of isomeric 3-{3-[2-(ethenyloxy)ethoxy]-2-hydroxypropyl}- and 5-{[2-(ethenyloxy)ethoxy]- methyl}-3-(2-hydroxyalkyl)oxazolidin-2-ones. If the initial oxazolidin-2-one contains two alkyl groups on C⁴, 3-{3-[2-(ethenyloxy)ethoxy]-2-hydroxypropyl}oxazolidin-2-ones are selectively formed.     

(R)-2-{[4-(3-甲氧基丙氧基)-3-甲基吡啶-2-基]甲基亚硫酰基}- 1H-苯并咪唑的合成

以2,3-二甲基吡啶为起始原料, 经过11步反应, 不对称合成了质子泵抑制剂的关键中间体: (R)-2-{[4-(3-甲氧基丙氧基)-3-甲基吡啶-2-基]甲基亚硫酰基}-1H-苯并咪唑. 研究了用手性高效液相色谱拆分对映体、测定产品光学纯度的方法, 结果表明目标产品的ee值达到99%. 通过IR, UV, MS以及1H NMR分析对重要中间体和目标产品进行了结构鉴定.     

~(18)F标记前体3'-甲氧基-7-对甲苯磺酰氧丙氧基槲皮素的合成

以槲皮素为起始原料,经酰化、醚化、苄醚化、脱苄、甲基化、水解6步反应合成了18F标记前体3'-甲氧基-7-对甲苯磺酰氧丙氧基槲皮素,其结构经1H NMR,13C NMR和HR-MS(ESI)确证。     

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 title compound was determined by X-ray single-crystal diffraction. The crystal belongs to the orthorhombic system, space group P212121, with a = 10.26...     

4-{[Mono/dimethyl(1,1'-biphenyl)-4-yl]oxy}phthalonitriles and Phthalocyanines Based on Them

4-{[Mono/dimethyl(1,1'-biphenyl)-4-yl]oxy}phthalonitriles have been obtained by nucleophilic substitution of nitro group in 4-nitrophthalonitrile. The prepared phthalonitriles have been used for the synthesis of tetra-4-{[mono/dimethyl(1,1'-biphenyl)-4-yl]oxy}phthalocyanines and their complexes with copper, cobalt, and zinc. Spectral characteristics and thermal stability of the prepared compounds have been investigated.     

Synthesis and reactions of {o-{[bis(dimethylamino)boryl]methyl}phenyl}diphenylphosphane

The new α,ω-[boryl(organyl)]phosphane o-Ph₂PC₆H₄CH₂B (NMe₂)₂ ( 10 ) was obtained in good yields from the reaction of CIB(NMe₂)₂ with o-Ph₂PC₆H₄CH₂Li(tmeda). Five derivatives of 10 were obtained by substituting the boron-bound amino groups by reactions with MeOH, BCl₃, HCl, and LiAlH₄, respectively, in particular, o-Ph₂(HCl)PC₆H₄CH₂BCl₂ (HNMe₂) ( 10 e ) which shows a unique P? H? Cl? H? N unit. Compound 10 and its derivatives were characterized by multinuclear NMR methods, mass spectra, and elemental analyses. In addition, the structure of 10 e · 1.5 C₆H₆ was determined by single crystal X-ray diffraction.     

Synthesis and structure of 1,10-phenanthroline bis{[2-(2-pyrrole)-methylimino]4-methylphenolato}nickel(II)

Summary Electrochemical oxidation of nickel in an acetonitrile solution containing 2-pyrrole-[N-(2-hydroxy-4-methyl-phenyl)methylimine] (H₂L) and 1,10-phenanthroline (phen) yielded Ni(HL)₂·phen, whose crystal structure was determined by XRD. The nickel atom has a distorted octahedral geometry, and is coordinated to the phenolic oxygen and imino nitrogen atoms of two Schiff base ligands. The i.r. and u.v.-vis. spectra of the complex are discussed and related to the structure.     

4-(4-{5-[(二苄胺基甲酰)-甲基]-2-庚基-4-羰基-噻唑-3}-丁基)苯甲酸的合成研究

报道一个新型胰岛素增敏剂4-(4-{5-[(二苄胺基甲酰)-甲基]-2-庚基-4-羰基-噻唑-3}-丁基)苯甲酸的合成方法. 该化合物以对碘苯甲酸为原料, 经过羧基的保护、Heck反应、还原反应、Ing-Mnske反应、噻唑环合成、酰胺制备和羧酸保护基解除等一系列反应, 通过对反应条件的优化, 高产率合成4-(4-{5-[(二苄胺基甲酰)-甲基]-2-庚基-4-羰基-噻唑-3}-丁基)苯甲酸, 并对其中间体对碘苯甲酸叔丁酯的合成方法进行研究.     

2-(Tributylstannyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indole: Synthesis and use as a 1H-indol-2-yl-anion equivalent

Pd-Catalyzed reaction of 2-(tributylstannyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-indole ( 5 ) with a variety of aryl, heteroaryl, vinyl, and allyl halides provides an efficient entry to the corresponding cross-coupled products (see Table).     

Photophysical and Photoelectric Properties of 2—{[4—（N—Hexadecyl—N—methylamino）phenyl]methylene}—propanedinitrile

2-{[4-(N-Hexadecyl-N-methylamino)phenyl]methylene}-propanedinitrile(HMAPN) with typical donor-π-acceptor(D-π-A）structure was synthesized.It could be easily assembled into stable films by LB technique.The photophysical properties of HMAPN were investigated in solution and on LB films.The photoelectric properties of HMAPN were examined and the anodic photocurrent of the ITO electrode modified by the monolayer LB film of HMAPN was measured as 835 nA/cm^2 under the white light of 218.2 mW/cm^2 without bias voltage.The effects of light intensity,bias voltage on the photocurrent were discussed.The possible mechanism of the photocurrent formation was given.     

Synthesis and Crystal Structure of 1,4-Dimethyl-2,5-di{[2’-(3-pyridylmethylamino-formyl)phenoxyl]methyl}benzene Perchlorate

The title compound, 1,4-dimethyl-2,5-di{[2’-(3-pyridylmethylaminoformyl)phenoxyl]- methyl}benzene perchlorate (C36H36Cl2N4O12, Mr = 787.59), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal crystallizes in the orthorhombic system, space group Pbca with a = 14.366(4), b = 15.159(4), c = 16.443(5), V = 3580.9(17)3, Z = 4, Dc = 1.461 g/cm3, μ = 0.253 mm-1, F(000) = 1640, R = 0.0618 and wR = 0.1525 for 1615 observed reflections (I > 2σ(I)). In the structure of the title compound, a two-dimensional supramolecular layer is formed via intermolecular hydrogen bonding interactions.