Synthesis of Dialkyl [1-Hydroxy-2,2-dimethyl-3-(dialkylamino)propyl]phosphonates

Russian Journal of General Chemistry -     

Reactions of Selenobenzamide and Alkyl Halides. Synthesis of Dialkyl Selenides and Diselenides

In the absence of base, the reaction of selenooenzamide with alkyl halides gives the dialkyl diselenides as the major product. While the reaction of selenobenzamide and an alkyl halide is carried out in a 1:2 molar ratio and in the presence of strong base, the dialkyl selenides predominate.     

HO-Modification of Dialkyl [3-(Dialkylamino)-1-hydroxy-2,2-dimethylpropyl]phosphonates

Russian Journal of General Chemistry -     

N-糖基硫代亚脲基—(硫代)磷酰胺二芳基和二烷基酯的合成

二芳氧基磷酰肼(2a，2b)或二乙氧基硫代磷酰肼(4)与糖基异硫氰酸酯(5a-5b) 反应，生成相应的N-糖基硫代亚脲基—磷酰胺二芳基酯(6a-6d,7a-7d)和N-糖基硫 代亚脲基—硫代磷酰胺二乙基酯(8a-8d)．     

5-甲基-2(1H)吡啶酮的合成

以5-甲基-2-氨基吡啶为起始原料,通过重氮盐水解反应,合成了5-甲基-2(1H)吡啶酮,并对其合成工艺进行了研究,其结构经IR确证。     

Features of Reaction of Dialkyl Perfluoroadipic and Perfluoropimelic Acids with Alkyl(Aryl) Methyl Ketones

Reaction of dialkyl esters of perfluoroadipic and perfluoropimelic acids with ketones form diketo esters. The possibility of cyclization of the products is discussed.__________Translated from Zhurnal Obshchei Khimii, Vol. 75, No. 2, 2005, pp. 318–321.Original Russian Text Copyright © 2005 by Chapurkin, Litinskii, Baklanov, Leont’eva.     

The Synthesis and Reactions of Dialkyl 1-Vinylvinyl-Phosphates

3,4-Dichlorobutanone reacts with trialkyl phosphites to give dialkyl 1,3-butadien-2-yl phosphates. Their structures were determined by spectroscopic methods and various chemical reactions.     

烷基膦酸二烷基酯的固—液相转移催化合成及其阻燃性能

烷基膦酸二烷基酯的固－液相转移催化合成及其阻燃性能王筱梅＊杨平蔡庆华鲍猛（山东建筑材料工业学院应用化学系济南２５００２２）关键词烷基膦酸二烷基酯，合成，相转移催化，阻燃性１９９６－０８－１２收稿，１９９７－０３－０３修回烷基膦酸二烷基酯是一类具有实用...     

Synthesis and Crystal Structure of a Two-dimensional Cadmium Complex Based on Terephthalate and 1-Methyl-2,2'-bibenzimidazole

The title complex, Cd(MeHbibzim)(1,4-bdc)n (1, MeHbibzim = 1-methyl-2,2'- bibenzimidazole, 1,4-bdc = terephthalate), was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, space group C2/c with a = 9.822(4), b = 18.510(7), c = 22.372(9), β = 98.359(6)°, C23H16CdN4O4 , Mr = 524.81, V = 4024(3)3 , Z = 8, Dc = 1.733 g/cm3 , μ(MoKα) = 1.126 mm-1 , F(000) = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections (Ⅰ > 2σ(Ⅰ)). X-ray diffraction analysis reveals that the Cd atom is coordinated by two nitrogen atoms from the chelating MeHbibzim and three carboxyl oxygen atoms from three terephthalate ligands, thus forming a distorted square pyramidal coordination sphere, CdN2O3. Every two Cd atoms are linked together via two carboxyl groups into a dinuclear unit with Cd···Cd separation of 3.806(4). The dinuclear building units are linked by terephthalate ligands into two-dimensional layers, which are further aggregated into a 3D framework via hydrogen bonding interactions.     

The Facile Synthesis of Dialkyl 1-Aminoalkylphosphonates

During past several years we have been engaged in the synthesis of phosphono peptides, peptide analogues with phosphonic acid replacing C-terminal carboxylate moiety. They became increasingly important since they appeared useful as carriers of toxic aminoalkylphosphonic acids through bacterial cell wall^1–4 or into plant tissues.^1,5 The most succesful method for the synthesis of these peptides is the condensation of N-blocked amino acids with dialkyl 6,7 or diphenyl 8.9 esters of aminoalkylphosphonic acids followed by removal of protecting groups.     

A Convenient Synthesis of 1-(Dichloro-Pyrimidinyl Carbamyloxy) Alkyl Phosphonates

Abstract

In the study of the nucleophilic addtion reaction of dialkyl I-hydroxyphosphonate and dichloropyrimidinyl isocyanate. We found this reaction was a convenient way for the synthesis of 1-(substituted carbamy1oxy)alkyl phosphonatc derivative. Dialkyl 1 - hydroxyphos-phonate can be easily prepared by addtion of dialkylphosphitc to carbonyl compounds. 4,6-dicloro-2-isocyanato pyrimidine can be synthesized by the reaction of oxalyl chloride and 2-amino-4,6-dichloropyrimidine which can be obtained from 2-amino-4,6-dihydroxy pyrimidine.     

Synthesis and properties of 1-trimethylsilylthia-2,2-bis(trimethylsilyloxy)ethene

A. E. Arbuzov Institute of Organic and Physical Chemistry, Kazan Branch, Russian Academy of Sciences, 420083 Kazan. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 3, p. 766, March, 1992.     

Dialkyl (1-ethoxycarbonyl-2,2,2-trifluoro-1-phenylsulfonylaminoethyl)-phosphonates

A number of fluorine-containing ??-amino phosphonates of the general formula (RO)₂P(O)C(CF₃)(COOC₂H₅)NHSO₂Ph were obtained and found to irreversibly inhibit four serine hydrolases: acetyl- and butyrylcholinesterases, neuropathy target esterase, and carboxylesterase.     

2,2′-dihalo-bis(perfluorocycloalkenes): Part 1. Synthesis

An improved synthesis of 1-chloro-2-iodo-perfluorocycloalkenes and their copper coupled products, 2,2′-dichloro-bis(perfluorocycloalkenes) is reported. Mixtures of equal molar quantities of different chloroiodoperfluorocycloalkenes react with copper to give predominately the mixed coupled product. For example, 1-chloro-2-iodoperfluorocyclobutene and 1-chloro-2-iodoperfluorocyclopentene react with copper to give 2-chloro-1-[1′-2′-chlorohexafluorocyclopentenyl)]-tetrafluorocyclobutene in 70% yield. The 2,2′-dichloro-bis(perfluorocycloalkenes) react with potassium iodide in DMF to substitute one or both vinylic chlorine atoms by iodine. Copper coupling of 2,2′-diiodo-bis(perfluorocyclopentene) gives the cyclic tetramer perfluorotetracyclopentenocyclo-octatetraene, whereas 2-chloro-2′-iodo-bis(perfluorocyclopentene) and copper gives the linear tetramer 2,2?-dichlorotetrakis(perfluorocyclopentene).     

Synthesis of Derivatives of (4-Methyl-2-Quinolylthio)acetic and (4-Methyl-2-Quinolylthio)propionic Acids

An efficient synthesis has been developed for derivatives of (4-methyl-2-quinolylthio)acetic and (4-methyl-2-quinolylthio)propionic acids by the reaction of 4-methyl-2-thioxoquinoline with methyl methacrylate, the amide of methacrylic acid, acrylonitrile, ethyl bromoacetate, and ethyl acrylate. The hydrolysis of the resultant intermediates by (quinolylthio)acetic and (quinolylthio)propionic acids gave the corresponding acid products, which are also formed in the reaction of 4-methyl-2-thioxoquinoline with chloroacetic and acrylic acids. The reaction of 4-methyl-2-thioxoquinoline with allyl bromide was studied. The potassium permanganate oxidation of the resultant 2-allylthio-4-methylquinoline led to (4-methyl-2-quinolylthio)acetic acid.__________Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 403–406, April, 2005.     

Triphenylphosphine-Mediated Serendipitous Synthesis of Alkyl Cinnamates Through the Reaction of 3-Hydroxy-4-Methoxybenzaldehyde and Dialkyl Acetylenedicarboxylates

Abstract

Alkyl cinnamates are formed in fairly good yields from the reaction of dialkyl acetylenedicarboxylates and 3-hydroxy-4-methoxybenzaldehyde in the presence of triphenylphosphine.     

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.