Tris dimethylamino bismuth

All solvents must be appropriately dried and deoxygenated, all glassware should be dried in an oven and all manipulations should be carried out under an inert atmosphere. 

Li[NMe2] was prepared by condensing an excess of dimethylamine onto frozen n-BuLi and allowing the mixture to warm to room temperature with shaking following the procedure described by Chisholm et al.4 with the slight modification that immersion of the reaction flask in dry ice-propan-2-ol was omitted. 

A n-BuLi solution in hexanes (Aldrich) (1.77 M, 56.5 mL, 100 mmol) was transfered to a 500-mL, round-bottomed flask and frozen in liquid nitrogen. The flask was then evacuated and connected to a calibrated vacuum manifold. An excess of dimethylamine (HNMe2) was then condensed into the flask. The tap was closed and the mixture was allowed to warm slowly to room temperature while the flask was agitated (CARE ). Solid Li[NMe2] precipitates as the reaction proceeds. The volatiles are removed by vacuum and the white solid is pumped dry. 

This preparation is a modification of that reported by Ando et al.5 the main difference being that we did not find it necessary to reflux the reaction mixture or purify by distillation. 

Bi N(SiMe3)2 36 is an extremely air-sensitive, pale yellow microcrystalline compound that is very soluble in hydrocarbon and ether solvents. It is much less photosensitive than Bi(NMe2)3. H and 13C H NMR spectra at room temperature in d8-toluene show signals at 8 0.55 and 7.51 respectively. 

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Oxybis[ tris[4-(A, /7-dimethylamino)phenyl]bismuth dichloride 280 Phenylbismuth bis(dimethyldithiocarbamate) 122 Phenylbismuth bis(pyridine-l-oxide-2-thiolate) 123 Phenylbismuth diethoxide 121 Phenylbismuth ethanedithiolate 353 Phenylbismuth oxalate 122, 352... 

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