Hello,

I need to synthesize the Tris(triethylsilyl)bismuthane [(CH3CH2)3Si]3Bi. 

So far I tried an analogous method for Antimony described in DOI:10.1021/cm102904f. I assumed that the chemistry should be similar for bismuth. In the first step, I used Sodium naphthalenide and bismuth powder in DME in order to prepare Na3Bi alloy (reflux 2days). Then injected Chlorotriethylsilane followed by reflux for another two days. However, I noticed, that no Bismuth has been reacted (or maybe small fraction) after refluxing for two days, and I have some mess in flask now...

So my first assumption is that no Na3Bi alloy was formed, and the reaction did not proceed.  Because Bi is also black powder as resulting Na3Bi, I can't visually evaluate if the alloy is formed or not. 

So my question is maybe this method is not appropriate for bismuth? Or something wrong with the starting materials?

The alternative is to use NaK, but for safety reasons, I prefer to avoid NaK. 

All reactants used right after purchase, used bismuth powder (325 mesh) DME was purchased dry, stored under molecular sieves.

Any tips? suggestions?

I really need your help.