Re: ORGLIST:Bromination

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From: C. Oliver Kappe (oliver.kappe$##$uni-graz.at)
Date: Tue Aug 13 2002 - 10:47:20 EDT


Hello Jacob,

are you talking about a "Prolabo" instrument (previously supplied by
MERCK), is it a single-mode or multimode cavity?

Oliver

Jacob Zabicky schrieb:
>
> Hello Darren,
>
> What we have is batch. We use it for digestion of certain samples with
> harsh reagents. The configuration is such that, IMO, it can be made
> continuous tubular or backflow by drilling a couple of holes in strategic
> places and buying the appropriate tubing and joints. Maybe Merck has better
> ideas about that.
>
> All the best,
>
> Jacob
>
> At 13:29 13/8/2, Darren Rhodes wrote:
> >Is this a batch reactor or a continuous flow reactor ??? 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: Tuesday, August 13, 2002 1:26 PM
> >Subject: Re: ORGLIST:Bromination
> >
> >
> >> 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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> >> >> >
> >> >>
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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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> >> >> >
> >> >> >
> >> >> >_______________________________________________
> >> >> >ORGLIST - Organic Chemistry Mailing List
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> >> >> >
> >> >> >
> >> >> >_______________________________________________
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> >> >>
> >> >>
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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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> >> >>
> >> >>
> >> >>
> >> >
> >> >_______________________________________________
> >> >ORGLIST - Organic Chemistry Mailing List
> >> >Website / Archive / FAQ: http://www.orglist.net
> >> >To post a message (TO EVERYBODY) send to everybody$##$orglist.net
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> >>
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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
> >> 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
> >>
> >>
> >>
>
> 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
>
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-- 
C. Oliver Kappe
Institute of Chemistry      
Karl-Franzens-University Graz    Phone: +43-316-3805352
Heinrichstrasse 28, A-8010 Graz  Fax: +43-316-3809840
AUSTRIA                          e-mail: oliver.kappe$##$uni-graz.at
http://www-ang.kfunigraz.ac.at/~kappeco
_______________________________________________
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