No abstract

No abstract

No abstract

The method reported here utilizes the reaction between sulfur dichloride and N-(trimethylsilyl) sulfinylamine and gives a 68% yield of bis (sulfinylamino) sulfide conveniently. The other product, trimethylchloro-2MesSiNSO + SC12->-S(NSO)2 + 2Me3SiCl silane, was found to be an excellent recrystallization solvent for the amino sulfide. Benzene had been used previously.5The large, yellow rhombic crystals of the product were sensitive to traces of moisture. They could be conveniently handled in an atmosphere of dry nitrogen. The sample went red on heating and appeared to boil after melting, as previously reported.2 The infrared spectrum in carbon disulfide contained two major peaks at 1184 and 988 cm-1, attributable to the asymmetric and symmetric stretching vibrations of the sulfinylamino group.7Experimental Section Sulfur dichloride was purified by distillation in the presence of 10% of phosphorus trichloride,8 which inhibits disproportionation into sulfur monochloride and chlorine; the distillate was promptly used.N-(Trimethylsilyl )sulfinylamine was prepared in 88% yield according to the method of Scherer and Horning9 from tris-(trimethylsilyl)amine10 and thionyl chloride. The fraction boiling at 108°, n2°D 1.4254, was used.Bis (sulfinylamino) Sulfide.-In one experiment, 41.4 g (0.307 mol) of the silylsulfinylamine was placed in a 100-ml two-necked flask, fitted with a reflux condenser, and a 50-ml dropping funnel fitted with a by-pass. The whole apparatus was flushed with and maintained under an atmosphere of dry nitrogen, and 14.5 g (0.145 mol) of sulfur dichloride was slowly added to the sulfinylamine, with stirring. The reaction was exothermic, and fine, yellow' crystals w'ere deposited. The mixture was heated under reflux for 48 hr to ensure complete reaction. Long, yellow' needles formed on cooling and the liquid was then pumped off, trapped (30.2 g), and redistilled to yield trimethylcholorosilane (26.5 g, 87%), bp 57°, «25d 1.3864.The yellow crystals were dissolved in 50 ml of hot trimethylchlorosilane, recrystallized, and filtered under a dry nitrogen atmosphere. They were w'ashed with a little cold trimethylchlorosilane and all traces of solvent were pumped off over a period of 3 hr. The crystals melted in sealed tube at 100-101°( lit.4 mp 100.7°) (14.9 g, 68%).

No abstract