Re: ORGLIST:Bromination

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From: Jacob Zabicky (zabicky$##$bgumail.bgu.ac.il)
Date: Tue Aug 13 2002 - 08:26:10 EDT


Hello,

We have a microwave reaction system, with vessels of PTFE that withstand 40
bar. The equipment, including the oven, was supplied by

E. Merck
64271 Darmstadt
Germany

All the best,

Jacob

At 15:07 11/8/2, Darren Rhodes wrote:
>A couple of UK companies (Production Techniques Ltd, 13 Kings Road, Fleet,
>Hampshire, Enlgand GU13 9AU tel 01252 616757 facs 01252 615818 and Cowie
>Technology tel 01642 599190 facs 01642 596810) should be able to supply you
>with suitable PTFE vessels.
>
>Does anyone know the name and contact number of the people in Jenna
>(Germany) who are currently using lab scale microwave reactors????
>
>Darren.
>
>
>----- Original Message -----
>From: "Jacob Zabicky" <zabicky$##$bgumail.bgu.ac.il>
>To: "Darren Rhodes" <drhodes$##$globalnet.co.uk>;
><suzukicar$##$belais.freesurf.fr>; <everybody$##$orglist.net>; "Jacob Zabicky"
><zabicky$##$bgumail.bgu.ac.il>
>Sent: Sunday, August 11, 2002 6:51 AM
>Subject: Re: ORGLIST:Bromination
>
>
>> Hello again,
>>
>> If we come to microwave reactors, as Darren suggested, ultrasound is also
>> a possibility. IMO in both cases you will need a specially designed
>vessel,
>> both to allow inflow of energy to the reaction mixture and to avoid
>outflow
>> if the deletereous bromine vapors.
>>
>> All the best,
>>
>> Jacob
>>
>> At 13:15 8/8/2, Darren Rhodes wrote:
>> >It would be interesting to this sort of thing under microwave conditions
>...
>> >This should bring down your reaction time and if you wanted to do the
>work
>> >on a larger scale you could use a continuous flow microwave reactor ...
>For
>> >the batch microwave work talk to http://www.personalchemistry.com/ (the
>web
>> >page seems a bit bloated but it should give you contact details). For
>the
>> >continuous flow ... maybe the personalchemistry people again ??? Perhaps
>> >someone else on the list could give appropriate details and refs and
>perhaps
>> >their own experiences of these techniques .....
>> >
>> >Darren.
>> >
>> >----- Original Message -----
>> >From: "Jacob Zabicky" <zabicky$##$bgumail.bgu.ac.il>
>> >To: <suzukicar$##$belais.freesurf.fr>; <everybody$##$orglist.net>
>> >Sent: Thursday, August 08, 2002 12:32 PM
>> >Subject: Re: ORGLIST:Bromination
>> >
>> >
>> >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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>> >Prof. Jacob Zabicky
>> >Institutes for Applied Research
>> >Ben-Gurion University of the Negev Private: POB 12366, Beer-Sheva
>> >84863
>> >POB 653, Beer-Sheva 84105, ISRAEL Tel. +972-8-6496792
>> >http://profiler.bgu.ac.il/site/main.cfm
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>> >
>> >
>> >_______________________________________________
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>> x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x
>> Prof. Jacob Zabicky
>> Institutes for Applied Research
>> Ben-Gurion University of the Negev Private: POB 12366, Beer-Sheva
>84863
>> POB 653, Beer-Sheva 84105, ISRAEL Tel. +972-8-6496792
>> http://profiler.bgu.ac.il/site/main.cfm
>> Tel. +972-8-6461271/6461062/6472754
>> Fax. +972-8-6472969
>> x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x-x
>>
>>
>>
>
>_______________________________________________
>ORGLIST - Organic Chemistry Mailing List
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Prof. Jacob Zabicky
Institutes for Applied Research
Ben-Gurion University of the Negev Private: POB 12366, Beer-Sheva 84863
POB 653, Beer-Sheva 84105, ISRAEL Tel. +972-8-6496792
http://profiler.bgu.ac.il/site/main.cfm
Tel. +972-8-6461271/6461062/6472754
Fax. +972-8-6472969
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_______________________________________________
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