Improved synthesis of the radical source bis[2,2,6,6-tetramethylpiperidyl-(1)]-disulfide and photoinduced reactions with M2(CO)10 (M=Mn, Re)
作者:Peter Jaitner、Karl Jäger、Astrid Dorfer、K.-E. Schwarzhans
DOI:10.1016/s0022-328x(00)00847-0
日期:2001.3
An improved synthesis of bis[2,2,6,6-tetramethylpiperidyl-(1)]-disulfide ((tmps)2) in moderate yield is reported. Reaction of N-(trimethylsilyl)-imidazole with S2Cl2 gives N,N′-dithiobisimidazole and trimethylsilylchloride. The disulfide undergoes exchange of the heterocycle wth 2,2,6,6-tetramethylpiperidine and yields bis[2,2,6,6-tetramethylpiperidyl-(1)]-disulfide and imidazole. This synthesis offers
报道了一种中等产率的双[2,2,6,6-四甲基哌啶基-(1)]-二硫化物((tmps)2)的合成方法。的反应ñ - (三甲基硅烷基) -咪唑以S 2氯2给出Ñ,Ñ '-dithiobisimidazole和三甲基氯硅烷。二硫键与2,2,6,6-四甲基哌啶进行杂环交换,生成双[2,2,6,6-四甲基哌啶基-(1)]-二硫键和咪唑。该合成提供的优点是仅产生痕量的双[2,2,6,6-四甲基哌啶基-(1)]-三硫化物。二聚体化合物[M(CO)4 tmps] 2的合成及光谱性质描述了通过(tmps)2与M 2(CO)10的混合物的紫外线照射获得的(M = Mn,Re)(M = Mn,Re)。