From: Jacob Zabicky (zabicky$##$bgumail.bgu.ac.il)
Date: Thu Aug 08 2002 - 07:32:12 EDT
Hello Bel,
The pressure in the vessel will be somewhat lower than 4 bar. If your
reaction mixture is over a couple of mL, you should carry out the process
in a Teflon-lined pressure vessel. If you can do it in small batches,
then you can prepare thick-walled test tubes, of outer diameter not bigger
than say 10 mm, place your mixture, freeze it with ice-salt or other
cooling medium (below -10C), and seal the tubes while slightly evacuating
at the end.
You can place the tubes in boiling water or in a temperature-controlled
heating block, all this, of course in a well protected hood. Thick-walled
tubes of small diameter withold some pressure quite well.
Good luck,
Jacob
At 16:23 7/8/2, Bel wrote:
>Dear all,
>
>I would like to know If any has experience with bromination in harsh
>conditions, using sealed tube at high temperature. I found one procedure
>concerning the bromination of an electronically poor aromatic (pyridinium
>derivative) which must be done by heating during 3 days at 180C. The
>bromine’s boiling point is 58.7C, which means a very high pressure in the
>tube at 180C. So does anyone know how to make such reaction in a safe way,
>and which kind of tube may resist to such pressure?
>
>Regards
>
>Bel
>
>
>
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Institutes for Applied Research
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