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    • 6. 发明授权
    • Silicon-based blocking agents suitable for fluorous phase synthesis
    • 适用于氟相合成的硅基封闭剂
    • US06642403B2
    • 2003-11-04
    • US10288815
    • 2002-11-06
    • Barry C. ArklesYoulin PanGerald L. Larson
    • Barry C. ArklesYoulin PanGerald L. Larson
    • C07F704
    • C07F7/0876Y02P20/582
    • This invention relates to a series of fluoroalkylsilane compounds of formula I. These compounds are silylation reagents which enhance the solubility of the silylated products in fluorocarbon solvents for preferred use in fluorous phase synthesis. Use of these compounds protects fragile hydrogen groups and also provides for the straightforward separation of the ultimate reaction products though fluorous phase extraction. This invention also relates to a two-step process for making compounds of formula I. The process comprises reacting an alkyldialkoxysilane with a perfluoroalkyl-substituted silane to produce a perfluoroalkyl-substituted dialkylsiloxyalkylsilane intermediate; and reacting the intermediate with halogen.
    • 本发明涉及一系列式I的氟代烷基硅烷化合物。这些化合物是甲硅烷基化试剂,其增强甲硅烷基化产物在氟碳溶剂中的溶解度,以优选用于氟相合成。 这些化合物的使用保护脆性氢基团,并且还提供通过氟相萃取直接分离最终反应产物。 本发明还涉及制备式I化合物的两步法。该方法包括使烷基二烷氧基硅烷与全氟烷基取代的硅烷反应以产生全氟烷基取代的二烷基硅氧烷基硅烷中间体; 并使中间体与卤素反应。
    • 10. 发明授权
    • Branched higher alkylsilanes
    • 支链高级烷基硅烷
    • US5874603A
    • 1999-02-23
    • US892595
    • 1997-07-15
    • Barry C. Arkles
    • Barry C. Arkles
    • B01D15/08B01J20/32C07F7/10C07F7/12C07F7/18C07F7/08
    • B01J20/3246B01J20/287C07F7/10C07F7/12C07F7/1836C07F7/184
    • A branched alkylsilane includes a branched hydrocarbon backbone which has a linear or branched alkylsilyl moiety extending asymmetrically from the backbone such that the backbone has a first portion and a second portion extending from the moiety. The second portion has two carbon atoms more than the first portion, and the alkylsilyl moiety includes at least one hydrolyzable group bound to silicon for reacting with a substrate. A method for preparing a branched alkylsilane useful for chromatographic applications includes the steps of preparing a vinylidene olefin by dimerization of an .alpha.-olefin and reacting it with a monomeric silane having a silicon-hydrogen bond in the presence of a metallic catalyst such that the silicon-hydrogen bond is added to the vinylidene double bond of the vinylidene olefin thereby converting the double bond to a single bond and bonding the silicon of the monomeric silane to the vinylidene olefin to form a branched alkylsilane.
    • 支链烷基硅烷包括具有从主链不对称延伸的直链或支链烷基甲硅烷基部分的支链烃主链,使得主链具有从该部分延伸的第一部分和第二部分。 第二部分具有比第一部分多两个碳原子,并且烷基甲硅烷基部分包括与硅键合的至少一个可水解基团以与基底反应。 制备可用于色谱应用的支链烷基硅烷的方法包括以下步骤:通过α-烯烃的二聚制备亚乙烯基烯烃,并在金属催化剂存在下使其与具有硅 - 氢键的单体硅烷反应,使得硅 将氢键加入亚乙烯基烯烃的亚乙烯基双键,从而将双键转化为单键,并将单体硅烷的硅键合到亚乙烯基烯烃上以形成支链烷基硅烷。