organichem
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Butyllithium
Hey folks, I want to prepare some BuLi - preferably in cyclohexane.
I've read several papers dealing with the preparation of BuLi in inert solvents.
Some are using Li with 1% Na, others pure Li - then some reflux after addition
of the chloroutane, or sonication is applied.
Is there anyone who has synthesized BuLi himself?
I'd appreciate a working method, I can try myself...
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kristofvagyok
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We use BuLi prepared by Sigma, but long ago the prof. attempted to make it, since we got ~50kg of Li.
Some notes before you start to prepare it:
-BuLi reacts with almost everything, even with atmospheric nitrogen.
-While making it from bromobutane and lithium a suspension of lithium-bromide forms what slows down the reaction and it's really hard to separate from
the BuLi.
-Chlorobutane reacts really slowly.
-It ignites easily upon contact with air.
I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:
"You can’t become a chemist and expect to live forever." |
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AvBaeyer
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Unless you REALLY know what you are doing and have all the proper safety equipment at hand, this is not something anyone without good lab experience
should be fooling with. Even if you can make butyl lithium, you will still need to learn how to transfer and store it. I have made a number of
organolithium reagents in my career and it is not a trivial exercise.
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organichem
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Harzard notes are substantial for BuLi - but I'm used to work with the Schlenk-technique and with pyrophoric substaces, although not with BuLi yet
(somewhere I have to begin  )
My laboratory equipment is quite good and I've been doing home since for 7 years now (and I'm working in the chemical industries as well) 
I just wanted a more-detailed instruction how to prepare it and maybe some experiences with the synthesis?
I just started the preparation on a 90 mmol scale with US at RT expected conc. should be ~0.8 M (for the beginning)
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Dr.Bob
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I would suggest reading the article that popped up in Google from "The Preparation of n-Butyllithium" which gives some detail. Unfortunately, I can
only get the first page right now, but it gives most of the details.
http://pubs.acs.org/doi/abs/10.1021/ja01172a510
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leu
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Some articles on preparing lithium reagents are attached 
Attachment: ja01172a510.pdf (79kB)
This file has been downloaded 1212 times
Attachment: Preparation of Organolithium Reagents.pdf (256kB)
This file has been downloaded 647 times
Attachment: safe.handling.organolithiums.pdf (142kB)
This file has been downloaded 389 times
Chemistry is our Covalent Bond
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leu
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Some more articles related to butyllithium are attached
Attachment: ja00889a021.pdf (227kB)
This file has been downloaded 590 times
Attachment: ja01330a069.pdf (110kB)
This file has been downloaded 719 times
Attachment: ja01864a058.pdf (119kB)
This file has been downloaded 574 times
Attachment: ja01866a020.pdf (234kB)
This file has been downloaded 696 times
Attachment: ja01870a036.pdf (114kB)
This file has been downloaded 703 times
Chemistry is our Covalent Bond
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Methyl.Magic
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Why do you want to use BuLi ? because sometime BuLi can be substitued with less dangerous grignard -BuMgBr reagents
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