Diaryl thioketones are selectively reduced with ytterbium metal to diarylmethanethiols, diarylmethanes or tetraarylethylenes, via thiometallacycle intermediates which undergo electrophilic coupling at thiocarbonyl carbon and sulfur.
Process for the Preparation of (Aminoalkylamino)Alkyl Halides and Conversion to Amifostine
申请人:Samsel Edward G.
公开号:US20080275265A1
公开(公告)日:2008-11-06
The present invention relates to processes for the preparation of (ω-aminoalkylamino)alkyl halides, their conversion to S-ω-(ω-aminoalkylamino)alkyl phosphothioates, and purification of the crystalline products of the reaction. The preparation process for the (ω-aminoalkylamino)alkyl halides comprises contacting an appropriate alcohol with a brominating agent in the presence of a sulfone solvent under temperature and pressure conditions suitable to effect salt formation without subsequent premature precipitation. The process is especially useful for converting (ω-aminoalkylamino)ethyl alcohol to amifostine.
The present invention relates to the preparation of halogenated (ω-aminoalkylamino) alkyls, their conversion to S-ω- (ω-aminoalkylamino) alkylphosphothioates, and purification of the crystalline product of the reaction. Regarding the method. The process for the production of halogenated (ω-aminoalkylamino) alkyl is to contact a suitable alcohol with a brominating agent in the presence of a sulfone solvent under suitable temperature and pressure conditions to provide salt formation without subsequent precipitating. Comprising making. The method is particularly useful for converting (ω-aminoalkylamino) ethyl alcohol to amifostine.
PROCESS FOR THE PRODUCTION OF POLYARYLENE SULFIDE RESINS
申请人:IDEMITSU KOSAN CO., LTD.
公开号:EP1550685A1
公开(公告)日:2005-07-06
The present invention is a process for the production of polyarylene sulfide based resin, wherein in washing a polyarylene sulfide based resin with a mixed solvent of an aprotic organic solvent and water in a softened or molten state, the polyarylene sulfide based resin partially dissolved in the washing liquid is recovered, to be specific, the polyarylene sulfide based resin dissolved in the washing liquid is precipitated, separated and recovered by cooling the washing liquid after washing and/or adding water to the washing liquid, and it is reused. According to the present invention, capable of being provided is a process for the production of polyarylene sulfide based resin in which the polyarylene sulfide based resin formed by polymerization is scarcely lost in washing the above resin with a solvent.
The production process of the present invention for polyarylene sulfide is characterized by that in a process for continuously producing polyarylene sulfide by reacting a sulfur source with a dihalogenated aromatic compound in an aprotic organic solvent, it comprises at least one polymerization reaction step in which two phases of a polymer phase and a solvent phase are separated and in which the polymer phase corresponding to a dispersion phase is a dispersion phase comprising globular droplets and that an end terminator is used in the above polymerization reaction step. According to the present invention, a polymer can be prevented from being adhered onto a polymerization reaction bath to thereby make it possible to discharge a polymer phase and a solvent phase from the polymerization bath in a constant proportion; resultingly, a PAS composition (concentration) in the polymerization bath can always be maintained at a constant value; and polyarylene sulfide having a raised and stabilized molecular weight can continuously be produced.
本发明的聚芳基硫醚生产工艺的特点是,在通过硫源与二卤代芳香族化合物在非沸腾有机溶剂中反应连续生产聚芳基硫醚的工艺中,至少包括一个聚合反应步骤,在该步骤中,聚合物相和溶剂相两相分离,其中与分散相相对应的聚合物相是由球状液滴组成的分散相,并且在上述聚合反应步骤中使用了末端终止剂。根据本发明,可以防止聚合物附着在聚合反应槽上,从而使聚合物相和溶剂相能够以恒定的比例从聚合槽中排出;因此,聚合槽中的 PAS 成分(浓度)可以始终保持在恒定值;并且可以连续生产出分子量得到提高和稳定的聚芳基硫醚。