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161.
《Phosphorus, sulfur, and silicon and the related elements》2013,188(11):2349-2356
Seven new 1-fluorinated-4-phosphopyrazoles 2 have been prepared in 60–94% yield by cyclization of N-(2′,2′,2′-trifluoroethyl) phosphonyl β-hydrazones 1 with triethyl orthoformate in the presence of acetic acid. The IR data, the 1H, 13C, 19F, 31P chemical shifts and coupling constants of the compounds 2 are reported. 相似文献
162.
163.
Jin Luo Shu Li Qiongwen Kang Yi Sun 《Phosphorus, sulfur, and silicon and the related elements》2013,188(12):1180-1186
AbstractSixteen novel 3-methylthio-5-substituted benzamido-6-arylamino-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4 (5H)-one derivatives (4a–p) were successfully synthesized from iminophosphoranes, aryl isocyanate, and substituted benzoylhydrazine. The structures of the title compounds were elucidated by FT-IR, 1H NMR, 13C NMR, and HRMS. Herbicidal activity of the compounds 4a–p against Brassica napus (rape), Echinochloa crusgalli (barnyard grass), Cucumis sativus (cucumber), and Triticum aestivum (wheat) were determined. The results showed that 5-(2-chlorobenzamido)-6-phenylamino-3-methylthio-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4 (5H)-one (4c) displayed remarkable inhibition activity against the stalk and root of rape with 100% inhibition rate at the dosages of 10?mg/L and 100?mg/L, and 5-(4-nitrobenzamido)-6-phenylamino-3-methylthio-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4 (5H) -one (4d) exhibited excellent activity against the stalk and root of barnyard grass with 100% inhibition rate at the same dosages. 相似文献
164.
Karim Akbari Dilmaghani Behzad Zeynizadeh Hadi Parasajam 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4):544-553
Abstract Various 3,4-dihydropyrimidin-2-(1H)-ones (DHPMs) and their sulfur derivatives were efficiently synthesized by a one-pot cyclocondensation reaction of aromatic and aliphatic aldehydes, β-dicarbonyl compounds and urea (or thiourea) in the presence of sulfuric acid immobilized on activated charcoal (133% w/w). The reactions were carried out in refluxing n-hexane-acetonitrile (2.5:0.5 mL) within 5–150 min to give 3,4-dihydropyrimidinones (or thiones) in high to excellent yields (81–97%). 相似文献
165.
Xiao-Bo Ma Jing-Lin Zhang 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):233-237
Abstract 1,3,2-Diazaphosphetidin-4-one derivatives were synthesized. Their 1H NMR signals at ambient temperature displaed a broad doublet which eventually coalesced before becoming sharp upon warming, and the 13C NMR spectra also showed that the α-and β-carbons of the dialkylamino group were non-equivalent. The phenomena were ascribed to restricted rotation about the exocyclic P—N bond. 相似文献
166.
H. Lavayssiere G. Dousse J. Satge 《Phosphorus, sulfur, and silicon and the related elements》2013,188(1-4):411-422
Abstract Diffèrents modes de synthèse d'oxazolidones 1.2.4-7 et de dioxolonnes 8-11 germaniées sont décrites. La stabilité thermique de germadioxolonnes a été étudiée. La décomposition procède d'un méchanisme du type (2 + 2 + 1), avec ouverture du cycle et formation de germylène. La réactivité chimique des oxazolidones et dioxolonnes germaniées a été étudité. Des réactions d'échange avec des dérives organominéraux dichlorés conduit facilement et avec de bons rendements aux derives isologues, phosphorés(III). arseniés(III), soufrés. ou germaniés(IV). La réaction d'échange entre une dioxolonne germaniée et le dichlorogermylène nous a permis d'obtenir un nouveau germylène fonctionnel cyclique stable 20 qui a été caractérisé par spectrographie (RMN 1H. masse). Different synthetic ways for germaoxazolidones 1.2.4-7 or dioxolonnes 8-11 have been described. The thermal stability of germadioxolonnes has been studied. Decomposition occurs by a [2 + 2 + 1] ring opening with formation of germylene. The chemical reactivity of germaoxazolidones or dioxolonnes has been studied. Exchange reactions with dihalogenated covalent compounds occur readily lcading to phosphorus(III). arsenic(III). sulphur or germanium(IV) analogs. From dichlorogermylene, new stable fonctionnal cyclic germylene 20 is obtained and characterized. 相似文献
167.
Giovanna Delogu Ottorino De Lucchi Maria Paola Fois Giovanni Valle 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3-4):417-425
Abstract Ketimines la-d derived from ortho-aminosubstituted phenylthioethers were prepared in order to determine the degree of chirality transfer from the chiral auxiliary to the sulfur atom in the formation of the sulfoxide or to the α-carbon atom in the reaction of the anion with alkyl halides or benzaldehyde. Oxidation to the sulfoxide occurred with little or no asymmetric induction. The crystalline benzyl sulfone 4c was deprotonated by alkyllithium or Grignard reagents and reacted with alkyl halides and benzaldehyde, in all cases with little to fair transfer of chirality. The major diastereoisomer from methylation of the anion of 4c with methyl iodide, was isolated, and afforded the enantiomerically pure amine 5 after removal of the chiral auxiliary. An X-ray structure determination of 4d allowed the assignment of the absolute configuration of the asymmetric carbon and revealed that the conformation of the ketimine in the crystal state is not homogeneous. 相似文献
168.
Paula M. Marcos Sandra Félix Jose R. Ascenso Manuel A.P. Segurado Besma Mellah Rym Abidi 《Supramolecular chemistry》2013,25(4):285-297
The binding properties of three p-tert-butyldihomooxacalix[4]arene tetraketone derivatives (tert-butyl 2b, adamantyl 2c and phenyl 2d) in the cone conformation and one derivative (methyl 2a) in a partial cone conformation, towards alkali and alkaline earth metal cations have been established by extraction studies of metal picrates from water into dichloromethane, stability constant measurements in methanol and acetonitrile, and by 1H NMR spectrometry. Transport experiments of metal picrates through a dichloromethane membrane were also performed. The results are compared to those obtained with closely-related calix[n]arene derivatives (n = 4 and 5) and discussed in terms of the substituents, size and conformational effects. Methylketone 2a is a poor binder for all the cations studied, due to its partial cone conformation. Ketones 2b, 2c and 2d show high extraction and complexation levels for the alkali cations, with similar profiles and preference for K+ and Na+ (plateau selectivity). Towards alkaline earth cations, these ketones show a strong peak selectivity for Ba2+ in extraction, but a plateau selectivity for Ca2+, Sr2+ and Ba2+ in complexation. The nature of the substituent attached to the ketone function has some influence on their binding properties, with phenylketone 2d being a slightly weaker binder than ketones 2b and 2c. 1H NMR titrations confirm the formation of 1:1 complexes between the ketones and the cations studied, also indicating that they should be located inside the cavity defined by the phenoxy and carbonyl oxygen atoms. Ketones 2b, 2c and 2d show transport rates that do not follow, in general, the same trends observed in extraction and complexation. 相似文献
169.
Jean Guillon Jean-Michel Leger Cecilia Dapremont Lou Apollonia Denis Pascal Sonnet Stéphane Massip 《Supramolecular chemistry》2013,25(5):319-329
The synthesis of new 25,27-dialkyloxy-5,17-diarylcalix[4]arenes-crown-6 1a–f in 1,3-alternate conformation by Suzuki cross-coupling reaction is reported. Their conformation was determined using 1H, 13C, 2D NMR and ROESY analysis, and X-ray crystallography. Extraction experiments using a two-phase solvent method involving sodium, potassium or cesium picrate showed good extraction of the cesium cation. The X-ray crystal structures of 1,3-alternate 25,27-dipropoxy-5,17-diphenylcalix[4]arene-crown-6 ether 1a and its cesium picrate complex were established. Solid-state data were used to determine the complexation behavior of these new ligands. The efficiency of calixarenes 1a–f for cesium ion extraction could be ascribed to the rigidity and flatness linkages caused by the aryl groups at the lower rim of the aromatic moieties in the calixarene skeleton. In addition, the introduction of these aromatic moieties in positions 5 and 17 enhanced the solubility of the metal complexes in organic media. 相似文献
170.
《Green Chemistry Letters and Reviews》2013,6(1):13-17
Abstract Amberlyst-15® (H+) resin catalyzes efficient one-pot solvent free Prins cyclization of an aldehyde and a homoallylic alcohol to yield dihydropyrans and 4-hydroxytetrahydropyrans. The products, which display interesting olfactory property, are obtained under mild condition and by simple work up. The recovered resin can be used repeatedly . 相似文献