- Production method of alkyl phosphine (by machine translation)
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The method comprises the following steps: mixing phosphine and propylene in a solvent, then adding the photocatalyst, reacting the phosphine with propylene in 20 - 50W light irradiation, and having short reaction time, relatively simple reaction time, relatively simple post-treatment, relatively simple post-treatment, and higher yield and purity of the product compared with the prior art, and the reaction time is shorter. 1 - 12h 0 °C - 50 °C. The method comprises the following steps of: carrying out free radical reaction at a temperature and a normal pressure. (by machine translation)
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Paragraph 0044-0059
(2020/12/10)
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- Synthesis, structure and reactivity of sulfur-rich [Fe(L1)(L2)('tpS4')] complexes with rigid [Fe('tpS4'] cores and σ-π co-ligands ('tpS4'2- = 1,2-bis(2-mercaptophenylthio)phenylene(2-); L1 L2 = CO, PR3, NO)
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Optimisation of synthesis and purification steps has made the new ligand 'tpS42- available in preparative amounts. Treatment of FeC12.4H2O with 'tpS4-Li2 or 'tpS4'-Na2 yielded [Fe('tpS4')] (1), which in the solid state and in the absence of co-ligands probably trimerises to give paramagnetic [Fe('tpS4')]3. The [Fe('tpS4')] fragment displays helical coordination of the 'tpS4'2 -ligand and binds σ-π ligands such as CO, NO and phosphanes to give diamagnetic 18-valence-electron complexes of general formula [Fe(L1)(L2) ('tpS4')]. The cis-dicarbonyl complex [Fe(CO)2('tpS4')] (2) is labile and readily dissociates CO to give dinuclear [Fe(CO)('tpS4')]2 (3). Simultaneous coordination of CO and phosphanes yielded [Fe(CO)(PR3)('tpS4')] with R = Me (4), Et (5), Pr (6) and Bu (7), but it proved impossible to obtain analogous complexes with bulky PPh3 or PCy3 ligands. Bis(phosphane) complexes could be obtained only with PMe3 and the bidentate dppe, which yielded [Fe(PMe3)2('tpS4')] (8) and [Fe(dppe)('tpS4')] (11). Alkylphosphanes with longer alkyl substituents, such as PnPr3 and PnBu3, gave the labile derivatives [Fe(PR3)2-('tpS4')] with R = nPr (9) and nBu (10). Complexes 9 and 10 reversibly dissociate one PR3 ligand, yielding diamagnetic [Fe(PR3)('tpS4')] fragments. These findings explain the decisive and hitherto inexplicable influence of PPr3 and PBu3 ligands upon the stabilisation of N2H2 in the diazene complexes [μ-N2H2{Fe(PR3) ('tpS4')}2] with R = Pr, Bu. Treatment of [Fe('tpS4')] (1) or [Fe(CO)('tpS4')]2 (3) with NO or NO+ yielded [Fe(NO)2('tpS4')] (12). The molecular structures of 3, 4, 7 and 8 were determined by X-ray structure analysis. Spectroscopic and structural results indicate that the differences in reactivity between [Fe(L1)(L2)('tpS4')] and homologous [Fe(L1)(L2) ('S4')] complexes can be traced back to subtle electronic and structural effects. Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003).
- Sellmann, Dieter,Blum, David C. F.,Heinemann, Frank W.,Sutterial, Joerg
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p. 418 - 426
(2007/10/03)
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- Method for manufacturing acryloxypropysilane
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A method to manufacture acryloxypropylsilane to a high degree of purity is achieved by hydrosilation of (A) allyl acrylate or allyl methacrylate by (B) a hydrosilane compound, using (C) a platinum-containing compound as the catalyst and (D) an organic phosphorus compound as the promoter. The acryloxypropylsilane product is expressed by General Formula I where R1 represents a hydrogen or methyl group, R2 represents a hydrolyzable group, R3 represents an aryl, alkenyl or aryl group of carbon number 1-12, and n is 0, 1, 2, or 3.
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- Electrosynthesis and chemical properties of hexaalkyldiphosphonium salts
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Electrochemical oxidation of trialkylphosphines on the background of sodium perchlorate or tetraethylammonium tetrafluoroborate allows synthesis of a new class of organophosphorus compounds, hexaalkyldiphosphonium salts. A mechanism of the electrosynthesis is proposed, which includes generation of radical cations R3P+? on the anode, their reaction with the starting phosphine to give a dimeric radical cation whose oxidation leads to the final product. The synthesized hexaalkyldiphosphonium salts readily react with compounds containing an active hydrogen atom, as well as with dialkyldisulfides, but do not react with aromatic or unsaturated compounds under normal conditions.
- Romakhin,Palyutin,Nikitin
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p. 905 - 910
(2007/10/03)
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