Synthesis of perfluorinated allylic compounds by radical allylation and their purification over fluorous reverse-phase silica
摘要:
A simple free-radical method for the preparation of a variety of perfluorinated allylic compounds has been developed starting from perfluoroalkyl iodides and allyltins. Allyltributyltin, methallyltributyltin and crotyltributyltin all proved to be useful For the transformation. The desired perfluorinated allylic compound was conveniently isolated from the crude mixture by solid-phase extraction with fluorous reverse-phase silica (FRPS). (C) 2001 Elsevier Science Ltd. All rights reserved.
A method of separating at least a first non-fluorous compound from a mixture of compounds including at least the first non-fluorous compound and a second fluorous compound includes: charging the of compounds to a non-fluorous solid (stationary) phase and eluting with a fluorous eluting fluid (mobile phase). In one embodiment, the non-fluorous solid phase is polar in nature. The method can further include a second phase elution with a suitable organic solvent. A method conducting a chemical reaction, includes: mixing at least a first fluorous compound and a second compound, the first fluorous compound differing in fluorous nature from the second compound; exposing the first mixture to conditions to convert at least one of the first fluorous compound and the second compound to give a second mixture containing at least a third compound, charging the second mixture to a non-fluorous solid phase; and eluting with a fluorous fluid
A method of separating at least a first non-fluorous compound from a mixture of compounds including at least the first non-fluorous compound and a second fluorous compound includes: charging the of compounds to a non-fluorous solid (stationary) phase and eluting with a fluorous eluting fluid (mobile phase). In one embodiment, the non-fluorous solid phase is polar in nature. The method can further include a second phase elution with a suitable organic solvent. A method conducting a chemical reaction, includes: mixing at least a first fluorous compound and a second compound, the first fluorous compound differing in fluorous nature from the second compound; exposing the first mixture to conditions to convert at least one of the first fluorous compound and the second compound to give a second mixture containing at least a third compound, charging the second mixture to a non-fluorous solid phase; and eluting with a fluorous fluid
Synthesis of perfluorinated allylic compounds by radical allylation and their purification over fluorous reverse-phase silica
作者:Ilhyong Ryu、Sergio Kreimerman、Tatsuro Niguma、Satoshi Minakata、Mitsuo Komatsu、Zhiyong Luo、Dennis P Curran
DOI:10.1016/s0040-4039(00)02153-5
日期:2001.1
A simple free-radical method for the preparation of a variety of perfluorinated allylic compounds has been developed starting from perfluoroalkyl iodides and allyltins. Allyltributyltin, methallyltributyltin and crotyltributyltin all proved to be useful For the transformation. The desired perfluorinated allylic compound was conveniently isolated from the crude mixture by solid-phase extraction with fluorous reverse-phase silica (FRPS). (C) 2001 Elsevier Science Ltd. All rights reserved.
US7364908B2
申请人:——
公开号:US7364908B2
公开(公告)日:2008-04-29
Reverse Fluorous Solid-Phase Extraction: A New Technique for Rapid Separation of Fluorous Compounds
作者:Masato Matsugi、Dennis P. Curran
DOI:10.1021/ol049040o
日期:2004.8.1
Fluorous-tagged compounds can rapidly be separated from organic (non-tagged) compounds by the new separation technique of reverse fluorous solid-phase extraction (r-fspe). In a reversal of the roles of solid and liquid phases in standard fluorous spe, a mixture is charged to a polar solid phase (standard silica gel) and then eluted with a fluorous solvent or solvent mixture. The organic components of the mixture are retained, while the fluorous components pass.