| 摘要 |
Two-stage preparation of highly pure organosilicon disulfans of formula Z-Alk-S2-Alk-Z (I) comprises (1) dissolving or suspending sulfur (S) and an anhydrous sulfide of formula Me2S (II) in 1:(0.2-0.9) molar ratio and treating the solution or suspension with an organosilicon compound of formula Z-Alk-Hal (III), with a molar ratio of (III) to sulfur of (1.2-2):1; and (2) adding more (II) after reaction, in an amount approximately equimolar to the total amounts of (II) and S used for reaction, and isolating (I); in which Z = -Si(R<1>)2R<2>, -Si(R<1>)(R<2>)2 or -Si(R<2>)3; R<1> = 1-5C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group optionally substituted by methyl (Me), ethyl (Et) or chlorine (Cl); R<2> = 1-5C alkoxy, 5-8C cycloalkoxy, phenoxy or benzyloxy; Alk = a 1-10C divalent, saturated linear or branched hydrocarbon group or -CH2-Phe-CH2-; Phe = phenylene; Me = ammonium, an alkali metal or one equivalent of an alkaline earth metal or zinc; Hal = Cl or bromine (Br). |
