六甲基二硅烷置于c4H15B11Br6Si,1,2-二氯乙烷,苯体系中,用> 95 %的收率获得一氯五甲基二硅烷 参考文献:芳烃离子催化全烷基化硅烷的卤代脱烷基化 标题:芳烃离子催化全烷基化硅烷的卤代脱烷基化 摘要:"有机硅"在自然界中并不存在,但现代化学很难想象没有硅与碳结合的情况.虽然含硅商品化学品(例如通过"直接工艺" 1,2,3,4产生的那些)看起来很简单,但选择性制备芳基取代和烷基取代(官能化)硅化合物(称为硅烷)并非易事.氯硅烷如 Me 4− N Sicl N ( N = 1-3) 以及 Sicl 4 ( N = 4) 是合成含硅分子的常见起点.然而这些方法常常遇到具有挑战性的分离问题5 .相反,具有四个烷基的硅烷被认为是合成的死角.在这里,我们介绍了芳烃离子催化的卤代脱烷基化反应,可有效地将 Me 4 Si 和相关的季硅烷转化为各种官能化衍生物.该反应使用烷基卤和芳烃(共)溶剂:烷基卤是卤化物源,最终与芳烃进行弗里德尔-克来福特烷基化以再生催化剂6,而芳烃离子则充当强布朗斯台德酸原脱烷基化步骤7 .例如,在硅药物前体的合成中,证明了自上而下的卤代烷基化方法相对于报道的自下而上程序的优势.此外,连接到烷基链上的相当惰性的me Doi:10.1038/s41586-023-06646-9
专利信息
专利号:US-8207366-B2 优先权日:2008-02-26 标题:Method for producing alkyl chlorosilanes from the residues of the direct synthesis of alkyl chlorosilanes 发明人:BOECK MANFRED; FUCHS PAUL; MAUTNER KONRAD 权利人:BOECK MANFRED; FUCHS PAUL; MAUTNER KONRAD; WACKER CHEMIE AG 摘要:High boiling residue from the direct synthesis of alkylchlorosilanes are converted in large part to monosilanes by heating the residue by passage of alternating current in a pressurized reactor.
专利号:US-6939984-B2 优先权日:2003-11-20 标 题 :Process for preparing alkylchlorosilanes from the residues of direct synthesis of alkylchlorsilanes 发明人:STRAUSSBERGER HERBERT 权利人:WACKER CHEMIE GMBH 摘要:The invention provides a continuous process for preparing alkylchlorosilanes from the residues of direct synthesis of alkylchlorosilanes which comprise liquid constituents with a boiling point of at least 70° C. at 1013 hPa and may also contain solids, with hydrogen chloride, by passing the residues at a temperature not above 200° C. and hydrogen chloride at a temperature higher than the latter into a reactor so that the resultant reaction temperature is from 400° C. to 800° C.
专利号:US-6344578-B1 优先权日:2000-08-10 标题 :Process for working up residues from the direct synthesis of organochlorosilanes 发明人:MAUTNER KONRAD; KOEHLER BERND; TAMME GUDRUN 权利人:WACKER CHEMIE GMBH 摘要:The invention relates to a process for preparing alkylchlorosilanes from the liquid constituents of the residues from the direct synthesis of alkylchlorosilanes which have a boiling point of above 70° C. at 1013 hPa and comprise disilanes, in which the residues are heated with hydrogen chloride and silicon at temperatures of at least 300° C., with at least 10% by weight of trichlorosilane and/or tetrachlorosilane, based on the weight of the alkylchlorosilanes formed, being formed at the same time.
专利号:US-5627297-A 优先权日:1995-04-10 标 题 :Process for cleaving the by-products of the direct synthesis of alkylchlorosilanes 发明人:GILBERT LAURENT; LAROZE GILLES 权利人:RHONE POULENC CHIMIE 摘要:The process for cleaving the heavy by-products derived from the synthesis of alkylchlorosilanes, in particular C1 to C6 alkylchlorosilanes, more particularly methylchlorosilanes, in particular for the cleavage of alkylchlorodisilanes, in particular methylchlorodisilanes having from one to five chlorine atoms, is carried out by treatment with hydrochloric acid in the presence of a catalytic system which comprises at least one metal phosphate, preferably associated with a basic impregnation compound. The metal phosphate may in particular correspond to the formula: M(XPO4)y in which M represents a metal chosen from: monovalent metals, in which case X is 2H and y=1 divalent metals, in which case X is H and y=1 trivalent metals, in which case X is absent and y=1 tetravalent metals, in which case X is: H and y=2 pentavalent metals, in which case X is 0 and y=1.
专利号:US-4289890-A 优先权日:1979-02-12 标 题:Synthesis of chloromethyldisilanes 发明人:GORDON ROY G 权利人:GORDON ROY G 摘要:1,2 Dichloro-1,1,2,2-tetramethyldisilane is synthesized in high yield and good purity starting from a crude mixture of chloromethyldisilanes formed as by-products in the manufacture of silicones. The new method uses less than half as much Grignard reagent as previous methods required. The synthesis can also be used to produce other haloalkyldisilanes such as chloropentamethyldisilane or 1,1,2 trichloro-1,2,2-trimethyldisilane.
专利号:US-4552973-A 优先权日:1984-03-23 标题 :Process for the preparation of dimethyldichlorosilane 发明人:FELDNER KURT; GRAPE WOLFGANG 权利人:BAYER AG 摘要:A process for the preparation of dimethyldichlorosilane from the low-boiling and high-boiling by-products of the direct synthesis of methylchlorosilane, comprising reacting methyltrichlorosilane simultaneously with the low-boiling components having a high content of methyl groups and with the high-boiling non-cleavable components, in the presence of a catalyst, at a temperature between about 250° C. and 400° C. and under a pressure of up to 100 bar.