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Chemistry Forums for Students => Organic Chemistry Forum => Topic started by: Janey on June 05, 2005, 08:27:57 AM

Title: How to synthesise 1-bromo-3-chloro-benzene?
Post by: Janey on June 05, 2005, 08:27:57 AM
Hello everyone  :),
we had a homework on benzene and this far I have solved all tasks left one:
finding a way to synthesize 1-bromo-3-chloro-benzene out of chlorobenzene.
But as far as I know chlorine is ortho-para directing  :-\
Is there maybe something I have to substitute to the benzene before substituting the bromine and remove it afterwards?
Unfortunetaly I can't find any such an example how to get it into meta position in one of my books *aarrrgh*
I'd be really happy if someone had an idea ^^
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: ksr985 on June 05, 2005, 09:45:16 AM
1 bromo 3 chloro benzene... i am assuming this is NOT asking for the most viable lab synthesis:

1. Nitrate benzene in mild conditions -----> nitrobenzene
2. Brominate the product-----> 1 nitro 3 bromo benzene
3. Prepare the diazonium salt with NaNO2/ HCl
4. Sandmeyer reaction( CuCl 60-100 degree C) will give the desired product.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: Janey on June 05, 2005, 10:01:05 AM
I'm afraid it is not, here it says chlorobenzene is the educt. :(
Thx for your reply, but there has to be another way...
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: movies on June 05, 2005, 01:22:05 PM
Ksr's route is certainly practical if benzene where the starting material.  It may be possible to use the same idea from chlorobenzene:

First, make the Grignard reagent from chlorobenzene and quench with an electrophilic NO2 source like tetranitromethane or N2O4.  That ought to give nitrobenzene and then you can go about ksr's route.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: GCT on June 05, 2005, 03:48:02 PM
Hello everyone  :),
we had a homework on benzene and this far I have solved all tasks left one:
finding a way to synthesize 1-bromo-3-chloro-benzene out of chlorobenzene.
But as far as I know chlorine is ortho-para directing  :-\
Is there maybe something I have to substitute to the benzene before substituting the bromine and remove it afterwards?
Unfortunetaly I can't find any such an example how to get it into meta position in one of my books *aarrrgh*
I'd be really happy if someone had an idea ^^

I imagine it can be accomplished with blocking groups, addition of bromine and subsequent removal.  I wonder, addition of nitro so that all ortho-para positions are filled, subsequent mild electrophilic addition of bromine...removal of nitro groups.  Movies, you think it can be done?

Have anyone of you considered a nucleophilic route, I'll need to review my text, but this might be a better alternative perhaps.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: Donaldson Tan on June 05, 2005, 04:33:41 PM
the gist is:
1. introduce a 3-directing substituent to benzene
2. add bromo group
3. substitute the 3-directing substituent with chloro

using -NO2 as the 3-directing group faciliates its subsequent substitution via the diazonium route.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: movies on June 05, 2005, 08:23:39 PM
I imagine it can be accomplished with blocking groups, addition of bromine and subsequent removal.  I wonder, addition of nitro so that all ortho-para positions are filled, subsequent mild electrophilic addition of bromine...removal of nitro groups.  Movies, you think it can be done?

Yeah, that was my first thought, but you would need a blocking group that would be an ortho-director and I don't recall any.  The most common one (sulfate) is a meta-director.

The SNAr route is interesting.  Might be a bit steppy though.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: dexangeles on June 06, 2005, 04:45:12 AM
guess what I found....

I believe the Zn/HCl is suppose to be the Clemmensen Amalgam of Zn(Hg), HCl
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: movies on June 06, 2005, 12:18:52 PM
guess what I found....

I think that only the second one would give the right product, don't you?  And that uses the wrong SM.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: GCT on June 06, 2005, 12:58:26 PM
Yeah, that was my first thought, but you would need a blocking group that would be an ortho-director and I don't recall any.  The most common one (sulfate) is a meta-director.

The SNAr route is interesting.  Might be a bit steppy though.

Not neccessarily SNAr, but nucleophilic substitution in general, I thought this would be a neat approach, although it may not turn out to be practical.

Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: dexangeles on June 06, 2005, 01:01:28 PM
I think that only the second one would give the right product, don't you?  And that uses the wrong SM.

isn't the Clemmensen amalgam a reducing agent?
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: ksr985 on June 06, 2005, 03:08:53 PM
looks like only the second one is correct.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: movies on June 06, 2005, 03:31:08 PM
isn't the Clemmensen amalgam a reducing agent?

Yes, in this case you would be reducing a nitro group to an amino group.  I don't think you actually need to use the amalgam for that reduction, just zinc dust and an acid.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: dexangeles on June 06, 2005, 05:17:26 PM
a) ok the nitro gourp is going to be para
then reduced to p-chloroaniline


b) the chlorine will be meta to the nitro group
then reduced to m-chloroaniline

is this correct so far?
what exactly does the 3rd synthesis step do?
with aniline in the mix this will control where the bromine is added right which would be ortho to it A and para to it in B, is this correct so far?

Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: dexangeles on June 06, 2005, 05:22:21 PM
ok I think I get it....it forms a diazonium salt. so it is B then


Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: Janey on June 07, 2005, 02:33:29 PM
Thank you very much folks :)
Even though I'm yet not totally sure, I think it will do for a start. Additionally, I asked a Doctor of Chemistry today, as soon as the reply returns I'll post it  ;)

And btw:
http://chemistry.boisestate.edu/rbanks/organic/mc/advanced%20problems/elec_sub_unsat/elec_sub_unsat.htm
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: hmx9123 on June 09, 2005, 05:44:45 PM
This is a bit late, but if you react a Grignard with an electrophilic source of NO2 +, you will wind up with a mixture of products (-NO2, -ONO).  You could concieveably do a Friedels-Crafts type nitration (so named by Olah), with a lewis acid catalyst like AlCl3 or TiCl4 and NO2Cl.  That's some nasty stuff, though.
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: Donaldson Tan on June 12, 2005, 04:52:37 PM
 :thmbup: to Dr HMX. LOL
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: Mitch on June 12, 2005, 06:30:56 PM
Not quite a doctor as yet. ;)
Title: Re:How to synthesise 1-bromo-3-chloro-benzene?
Post by: AWK on June 13, 2005, 01:37:16 AM
1. Nitration to m-dinitrobenzene
2. selective reduction of one nitro group (NaHS)
3. diazotization
4. Sandmayer's reaction
5. reduction
6. diazotization
7. Sandmayer's reaction