Novel Rearrangements of 2,3-Dimercapto-1-propanol Derivatives: Formation of Dialkyl Sulfide, Dialkyl Disulfide, and 1,2,3-Tris(alkylthio)propane

The base alkylation of 2,3-dimercapto-1-propanol with alkyl halides leads in good yield to 2,3-bis(alkylthio)-1-propanol and dialkyl sulfide. The reaction of 2,3-bis(alkylthio)-1-propanol with catalytic concentrated sulfuric acid proceeds with rearrangement to give 1,2,3-tris(alkylthio)propane and dialkyl disulfide. The rearrangement reaction takes place through a common intermediate thiaranium intermediate 8.     

Complexation Properties and Synthesis of 1,2-Bis(2,2'-bipyridinyl)ethylene and 1,2-Bis(2,2' -bipyridinyl)ethane Ligands with Cu(I)

l,2-Bis(2,2'-bipyridinyl)ethylene(1) ligand was synthesized by Wittig-Horner reaction and 1, 2-Bis(2, 2'-bipyridinyl)ethane(2) ligand(which can be obtained via another route ) was prepared by hydrogenation of (1). The formation of complexes of (1) and (2) with copper (I) has been studied. The influence of the different bridge chains (CH =CH, CH2CH2) on complexation is discussed on the basis of 1H NMR spectra. Keywords Dipyridine aldehyde, Dipyridine derivative, Copper complex     

Reaction of dialkyl H-phosphonates with azines and 1,2-bis(tert-butylimino)ethane

Acetaldehyde and butyraldehyde azines and 1,2-bis(tert-butylimino)ethane add only one molecule of dialkyl H-phosphonate at room temperature to form alkyl (-aminoalkyl)phosphonates. IR spectra of compounds obtained are discussed.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 2063–2065, August, 1996.     

Stereoselective Synthesis of Dialkyl 2-(Arylsulfonylamino)-3-(dialkoxyphosphoryl) Succinates by Reaction of Trialkyl(aryl) Phosphites,Dialkyl Acetylenedicarboxylates,and Arylsulfonamides

A three-component reaction of trialkyl(aryl) phosphites, dialkyl acetylenedicarboxylates, and arylsulfonamides is described as a simple and efficient route for the synthesis of dialkyl 2-(arylsulfonylamino)-3-(dialkoxyphosphoryl)-succinates in good yields.

Synthesis and Properties of Alkylene (Dialkyl) Dithiophosphate Derivatives of Thionyl Chloride

Alkylene (dialkyl) dithiophosphate derivatives of thionyl chloride of the general formula (S)SS(O)Cl and (RO)₂(S)SS(O)Cl where G = ─ CH₂(CH₃)₂CCH₂─, ─ CH₂CH₂CH(CH₃)─, ─ C(CH₃)₂CH₂CH(CH₃)─ and R = i-C₃H₇, have been synthesized by reacting thionyl chloride with alkylene/dialkyl dithiophosphates in a 1:1 molar ratio in refluxing benzene. A similar reaction in a 1:2 molar ratio yields the corresponding products of the type (S₂)₂S═O and [(RO))₂PS₂]₂S═O. It is interesting to note here that the sulfur atom of the thionyl chloride has been retained in the product, which is evidenced by sulfur analysis. The products thus obtained are light yellow colored semi solid (1:1 products) and orange colored liquids (1:2 products); and are soluble in common organic solvents. These new compounds have been characterized by elemental analysis, molecular weight measurements, and spectroscopic [IR and NMR (¹H and ³¹P)] studies. These compounds are found to be biologically active against bacteria S.aureus and E.coli.     

The Syntheses and Crystal Structures of cis-[Bis(diphenylphosphino)methane][1,2-bis(diphenylphosphlno)ethane] dicarbonylmolybdenum(O) and cis-[1,2-Bis(diphenylphosphino)ethane] [cis-1,2-bis(diphenylphosphino) ethylene]dicarbonylmolybdenum(0)

The title compounds, Mo(CO)₂(Ph₂PCH₂PPh₂)(Ph₂PCH₂CH₂PPh₂), Mo(CO)₂(dppm)(dppe) 1, and Mo(CO)₂(Ph₂PCH₂CH₂PPh₂)(Ph₂PCH = CHPPh₂), Mo(CO)₂(dppe)(cis-vpp) 2, were prepared from Mo(CO)₆ and the corresponding bidentate diphosphine ligands in n-decane under nitrogen atomosphere. Crystals of 1 are monoclinic, space group P 2₁/c, with a = 19.072(3), b = 11.348(3), c = 23.57(1) Å, β = 99.64(3)°, Z = 4, and the final residual R(F) = 0.044 for 4810 observed reflections; data of 2 are triclinic, space group P 1, with a = 12.091(3), b = 12.186(8), c = 18.934(5) Å, α = 96.93(4),β = 108.15(2), γ = 107.08(4)deg;, Z = 2, and the final residual R(F) = 0.058 for 4570 observed reflections. The distortion of compound 1 is more pronounced than that of compound 2, The two Mo-P lengths in the same bidentate chelate ligand for both compounds are different. Among them, the two larger Mo-P bond lengths for compound 2 are similar, but significantly different for 1.     

1,2-二(2-胺基苯氧基)乙烷银配合物的合成与晶体结构

本文采用配体1, 2-二(邻氨基苯氧基)乙烷(L)分别与AgPF6, AgCF3SO3, AgNO3和AgSbF6 进行配位反应,依次得到了四个配合物1 [Ag2(L)2(PF6)]、2 [Ag2(L)2(CF3SO3)2]、3 [Ag(L)NO3]n 和4 [Ag(L)2SbF6]n,并通过FTIR、元素分析、以及X射线单晶衍射等对配合物的结构与组成进行了表征。单晶衍射结果表明,配合物1和2为双核银(I)配合物,3和4为银(I)的配位聚合物。配合物1具有穴状结构,2经Ag?Ag键桥连两个配体形成扭曲的非平面结构。聚合物3的结构为一维(1D)“之”字链,4具有三维(3D)多孔的结构框架。在四个配合物结构中,相应的抗衡阴离子均未参与Ag(I)进行配位作用。     

Zinc(II) Complex with 1,2-Bis(2-Pyridyl-1,2,4-Triazol-3-yl)ethane and Dianions of 1-Hydroxyethane-1,1-Diphosphonic Acid

Russian Journal of Coordination Chemistry - The reaction of ZnSO4·7Н2О with 1,2-bis(2-pyridyl-1,2,4-triazol-3-yl)ethane (Н2L) and 1?hydroxyethane-1,1-diphosphonic acid...     

Dialkyl (Alkylene) Dithiophosphate Adducts of Anhydrous Stannous Chloride: Synthesis,Characterization, and Biological Activities

Abstract

Dialkyl (alkylene) dithiophosphate adducts of stannous chloride were synthesized by the reaction of anhydrous tin(II) chloride (SnCl₂) and dialkyl (alkylene) dithiophosphoric acid in a 1:1 molar ratio, under anhydrous reaction conditions, below 5 °C in a closed vessel. The newly synthesized adducts were characterized by physicochemical and spectroscopic techniques [FT-IR, NMR (¹H, ³¹P, and ¹¹⁹Sn), and mass spectrometry]. Coordination modalities have indicated a donor–acceptor interaction between sulfur and tin(II) moieties, where tin(II) acts as a Lewis acid. The adducts were found to have significant antibacterial activity against Escherichia coli and Pseudomonas aeruginosa, and antifungal activity against Aspergillus niger and Candida albicans.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

1,2—双[烷基（芳基）硫代]乙烷对银的萃取及其配合物

本文研究了1,2-双(正-丙基硫代)乙烷(BPrTE)、1,2-双(正-戊基硫代)乙烷(BATE)、1,2-双(正-辛基硫代)乙烷(BOTE)和1,2-双(苯基硫代)乙烷(BPTE)对银的萃取.讨论了硝酸浓度、稀释剂RS(CH_2)_2SR(L)中R基因对萃取银的影响.L可从大量贱金属和氯化物中定量地萃取银,银和配体可形成组成为Ag:L=2.5:1,2:1,3:2,1:1,2:3,1:2系列配合物.     

A Facile,One-Pot Synthesis of Azoic Compounds and Anthraquinone Derivatives Containing Dialkyl Phosphoryl Moieties in Multicomponent Reactions

Protonation of the reactive 1:1 intermediates produced in the reactions between triphenylphosphine and dialkyl acetylenedicarboxylates by 1-amino-anthraquinone or 1,5-diphenylcarbazone as a core dye leads to vinyl phosphonium salts, which undergo Michael addition with conjugate base of NH compounds to produce stable phosphorus ylides as novel dyes in fairly good yields. These ylides can exist in two geometrical isomers (Z) and (E) for 3, because the negative charge of the ylide moiety of these compounds are strongly conjugated with the adjacent carbonyl group. Rotation around the carbon–carbon double bond is slow in the (Z) and (E) geometrical isomers on the NMR time scale at ambient temperature. These compounds are assigned by their IR, ¹H, ¹³C NMR spectral data as well as their mass spectroscopic data.     

1，2-二（3-甲氧基4-羟基苯基）乙烷的产生条件与表征

1,2-二(3-甲氧基-4-羟基苯基)乙烷(1,2-Bis(4-hydroxy-3-methoxyphenyl)ethane),又名亚乙基双愈创木酚(Ethylenediguaiacol),双香兰素(Divanillyl),结构如图1中副产物.较早的报道[1,2,3]是从原木素降解得到,具有抗氧化及抗肿瘤作用[4].     

Synthesis and Crystal Structure of 1,2-Bis(1-phenyl-3-methylthio- 4-iminopyrazolo[3,4-d]pyrimidin-5-yl) ethane

1 INTRODUCTION As purine analogs, pyrzolo[3,4-d]pyrimidines have anti-tumor[1], antibacterial[2] and anti-leukemic activities[3,4]. Few of these, however, have been studied for pesticidal activity. It is reported that some substituted pyrzolo[3,4-d]pyrimidines have good fungicidal activity[5~7]. These prompted us to study pyrazolo[3,4-d]pyrimidines analogs further. It is shown that two possible products can be formed in the reaction of ethyl N-pyrazolylformimidate with alkylamines as sh…     

Trichloroisocyanuric Acid,as an Industrial Chemical,Promotes Transthioacetalization of Diacetals of 2,2-Bis (Hydroxymethyl)-1,3-propanediol and Cleavage of Thioacetals

Trichloroisocyanuric acid has been used as a mild, efficient, and new catalyst for transthioacetalization of diacetals of 2,2-bis (hydroxymethyl)-1,3-propanediol in CH 2 Cl 2 at room temperature. A clean, easy, and general method for efficient deprotection of thioacetals to their corresponding carbonyl compounds using trichloroisocyanuric acid/silica gel and water system also is described.     

Mo(CO)6催化炔烃三聚制备苯衍生物

Mo(CO)₆催化炔烃三聚制备了苯系衍生物, 并对催化剂用量和不同溶剂对产物收率的影响进行了考察, 推测了可能的催化反应机理.     

Synthesis of Derivatives of Pyrazolo[3,4-d]pyrimidines by Reaction of 3,5-Bis(dimethylaminomethylene)amino-4-methoxycarbonylpyrazole and 4-Cyanopyrazole with Amines

The reaction of 3,5-di-(N,N-dimethylaminomethylene)amino-4-methoxycarbonylpyrazole and 3,5-di-(N,N-dimethylaminomethylene)amino-4-cyanopyrazole with different amines occurs with formation of pyrazolo[3,4-d]pyrimidines. In some reactions, an excess of amines leads to their conversion to N,N-dimethylformamidine derivatives. The structure of the compounds obtained has been confirmed by ¹H NMR and ¹³C spectroscopy.     

2-Nitroguanidine Derivatives: V. Synthesis and Structure of 3,5-Bis(nitroamino)-1,2,4-triazole Salts. Acid–Base Properties of 3,5-Bis(nitroamino)-1,2,4-triazole

Heterocyclization of hydrazine-1,2-bis(N ²-nitrocarboximidamide) and salts derived therefrom provides a procedure for the synthesis of 3,5-bis(nitroamino)-1,2,4-triazole salts. The presence of two acceptor nitroamino groups conjugated with the triazole ring considerably enhances the acidity of 3,5-bis(nitroamino)-1,2,4-triazole (pK a¹= –2.0, pKa² = 4.8, pKa³ = 10.6) as compared to mononitroaminotriazole, so that formation of salts with the corresponding dianion becomes possible.     

Synthesis and Characterization of Novel Chiral (1R,2R)-1,2-Bis[5-(Aminomethylphospinic Acid)-1,3,4-Thiadiazol-2-YL]Ethane-1,2-Diols

Abstract

(1R,2R)-1,2-bis[5-(arylideneamino)-1,3,4-thiadiazol-2-yl]ethane-1,2-diol (2a–d) were synthesized by using appropriate aldehydes and (1R,2R)-1,2-bis(5-amino-1,3,4-thiadiazol-2-yl)ethane-1,2-diol (1) as a starting compound. Then, the phosphinic acid component (3a–d) were obtained from (2a–d) and hypophosporus acid. In addition, the structures of the novel chiral compounds (2a–d) and (3a–d) were confirmed by elemental analyses, IR, ¹H-NMR, ¹³C-NMR, and ³¹P-NMR spectra.

¹H NMR and ¹³C NMR spectra for 1, 2a, and 3a (Figures S1–S6) are available online in the Supplemental Materials.