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Topic: Any tips for working with n-BuLi outside the drybox?  (Read 6832 times)

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Offline nj_bartel

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Any tips for working with n-BuLi outside the drybox?
« on: August 25, 2009, 06:20:12 PM »
First time tomorrow!

Offline azmanam

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Re: Any tips for working with n-BuLi outside the drybox?
« Reply #1 on: August 25, 2009, 09:09:58 PM »
nBuLi is the most innocuous of the BuLi's.  By orders of magnitude.  Unless you're working with 25 M nBuLi, there's really nothing to worry about.

If you're using large volumes, you'll need to cannulate it out of the bottle into a flame-dried addition funnel, then add it to your rxn dropwise.  Otherwise, syringe away without fear.

also start here:
http://www.sigmaaldrich.com/etc/medialib/docs/Aldrich/Bulletin/al_techbull_al134.Par.0001.File.tmp/al_techbull_al134.pdf
Knowing why you got a question wrong is better than knowing that you got a question right.

Offline nj_bartel

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Re: Any tips for working with n-BuLi outside the drybox?
« Reply #2 on: August 25, 2009, 10:06:50 PM »
Thanks for the info  :)  The link refreshed some of the techniques I haven't used in a while.

Offline sjb

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Re: Any tips for working with n-BuLi outside the drybox?
« Reply #3 on: August 26, 2009, 03:15:39 PM »
Can't say I've ever used nBuLi in a drybox even using around 200ml of 2.5M in hexanes, though I have used NbCl5 in a "glovebox" - is that the same thing? Not the greatest of things to endow flexibility in my experience  :( As azmanam says, check out the Aldrich bulletins, and make sure you know were your exits / fire extinguishers etc are if necessary.

As an aside, correct me if I'm wrong, but it seems that many more procedures from the West side of the Atlantic seem to describe use of gloveboxes even for relatively air-stable reactions - does each (most) lab(s) have one, as this would be the exception rather than the rule in my (British) experiences...?

Offline Arctic-Nation

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Re: Any tips for working with n-BuLi outside the drybox?
« Reply #4 on: August 26, 2009, 05:32:20 PM »
I've done my master thesis and PhD thesis at the University of Leuven, and I do believe my group (synthesis, of course) had a glove box somewhere. Never used it, never knew of anyone actually using it.

I've done reactions with sec-BuLi in my fume hood, though for stuff like that I'd clean it out (a bit) and keep a coworker and a fire extinguisher nearby. The only accident with BuLi I've ever had was when a syringe with a glass plunger (these things are s#*$, but cheaper than teflon plungers, so there) overflowed onto my fingers. Judging from the limited heat generation, I still had some time to finish the transfer, so everything worked out fine in the end.
BuLi accidents were actually quite rare. LiAlH4, NaH, that's the stuff that burns. And Na metal of course. ;D

But gloveboxes? No thanks. When using dangerous chemicals, I like my freedom of movement. No need to make handling difficult.

Offline nj_bartel

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Re: Any tips for working with n-BuLi outside the drybox?
« Reply #5 on: August 26, 2009, 06:16:27 PM »
Well everything went fine :P

As far as gloveboxes (yeah, same thing), we have four in our lab, but we might be outside the norm as we do a lot of work with carbenes and radicals (some air stable, some not).

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