Re: ORGLIST:Details of Kipps-like generation of CO2?

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From: Thomas Høyer (alihoyer$##$mobilixnet.dk)
Date: Thu Aug 22 2002 - 16:00:45 EDT

I would use solid carbon dioxide. Break dry ice into lumps of a suitable size, wash it under argon in a flask with dry thf, and add the Grignard.

L. Brandsma's has written a few book on organometallic preparations, which contains reliable experimental details. These books are widely available.

Thomas Høyer

 
----- Original Message -----
From: "F.J. Lalor" <f.lalor$##$ucc.ie>
To: <everybody$##$orglist.net>
Sent: Wednesday, August 21, 2002 8:35 PM
Subject: ORGLIST:Details of Kipps-like generation of CO2?

> Ok - I am fully aware that this is a shamefully elementary question
> so no finger-wagging from the intellectual elite please 8-)
> For the purposes of a u/g lab experiment I need to generate small
> quantities of CO2 - preferably from a Kipps apparatus or something
> similar - to do a small-scale carbonation of PhMgBr. (Of course a
> cylinder would be easier but .... well, there are reasons). Now of
> course I know that all I need to do is drop sulphuric acid on calcium
> carbonate. Problem is I cannot find specific details anywhere. All
> the older practical textbooks in our library that might have
> described the experiment have long ago been dumped. So do I need
> conc. or dilute sulphuric acid? How do I dry the CO2 and avoid
> entrainment of acidic vapours? Any and all advice will be most
> gratefully appreciated.
> Regards -
> Fergus Lalor
> --
>
> --------------------------------------------------
> Dr. Fergus Lalor, Senior Lecturer, Chemistry Dept., University
> College, Cork, IRELAND.
> Telephone: 353-(0)21-4902317. Fax: 353-(0)21-4274097
>
>
>
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