[Ingeniosuccinimide]

Could anyone send me a link for a paper or name a book in which I could find a detailed procedure for purification of TMS-chloride?

I tried to google it and check from a couple of sources, but everything I found is that "it is done by fractional distillation over calcium chloride" which doesn't help a lot to a novice who never did that before. I need an example with a brief description, temperatures  and quantities used. Thanks.

[discodermolide]

It's a pretty labile compound containing small quantities of HCl from hydrolysis. Actually the purification is more bother than it's worth, just use it as it comes out of a fresh bottle and store under argon. I think it comes in one of those sure seal bottles from Aldrich so usual syringe methods work well here.

[Babcock_Hall]

I have fractionally distilled it.  I seem to recall having found information on how to purify it long, long ago, but I have not rediscovered it yet.  I can see some reason to reflux it before distilling it to drive off HCl.

[Ingeniosuccinimide]

Thanks for suggestions, but I can't use it directly, firstly because it's quite old, and secondly it is unlikely I will buy some as I do not have a permission from the supervisor (I'm using it to try a single completely new procedure in order to bypass one other known procedure which is not working).

I found a notice on purification in Chai, Armarego "Purification of Laboratory Chemicals" which is more of a Reference guide for experts, and it just gives a brief note without any examples of exact quantities, and this gives quite a headache to a novice. It's even more confusing when they say it should be "redistilled from calcium hydride", and they give no indications about the quantities. 

[Babcock_Hall]

I remember seeing that procedure one time; that was what I was looking for yesterday.  I may have even used it.  Usually one uses a small amount of CaH, relative to the amount of the solvent being distilled.  What I can say from experience is that old TMSCl should be fractionally distilled, because there was something else present when I distilled it.

[kamiyu]

1) The typical procedure I saw was distilled over CaH2. (The hydride here does not react with the Si center because of the mismatch of orbital size)

2) The reactivity depends on the steric hinderance around Si, so TMSCl is really reactive. The impurity is HCl, TMS-OH and TMS-O-TMS.

[Babcock_Hall]

TMS-O-TMS has a higher boiling point than does TMSCl; therefore, I would imagine that fractional distillation would separate them.