dormouse (Member)
04-21-00 00:23
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Author  Topic:   Rhodium:Toluidine 
Cheapskate
Member   posted 06-25-98 05:29 PM          
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In nitrating Nitrotoluene would one have to heat the mixture of toluene and nitric and sulfuric to get the reaction to progress?
When reducing nitrotoluene to toluidine is powered iron (or what) used and what conditions are needed to get this to happen?

Yes, I'm chemically challenged


mcdowell
unregistered   posted 06-25-98 08:37 PM           
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although it's rather expensive you can hypothetically get what you are trying to make at the local walmart in the pharmacy under diabetic testing kits its a hell of a lot safer to the procedure you mention involves TNT and is very dangerous if you don't know what you are doing it's not for the shade tree chemist!!!!!!!!!!!
 
CZ_74
unregistered   posted 06-25-98 08:54 PM           
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Use fuming HNO3 & conc. H2SO4 to make DNT from nitrotoluene(NT), keeping rxn temp below
60C. Reduce DNT to toluidine by SnCl2/HCl. |-)
CZ
 
mcdowell
unregistered   posted 06-27-98 07:34 PM           
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IF your going to use this synth set it up away from houses and people and stand clear this is a very unstable process(boom!)
 
Cheapskate
Member   posted 06-29-98 12:11 PM          
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I need a binding material that will not raise the ignition point of some thermite pellets I'm constructing for use as damp weather fire starters and I've seen nitro toluene used for this, so intriqued by Mcdowell's advice, and not a little worried about blowing my face off, but still curious (I'm not very smart apparently), I took my stuff and went away from civilization to try this.
I mixed 20ml of nitric with an equal volume of sulfuric in a round bottom flask and kept the reaction cool with an ice bath. I swirled the mix around until the reaction was not producing any heat anymore. Wearing a leather coat and pants with a safety shield over my face, I added dropwise 20 ml of toluene swirling each drop carefully and keeping the reaction cool. The toluene turned brown, then back to a yellowish. After the reaction mix had cooled completely, I had two distinct layers, the bottom one a light yellow and the top one a darker yellow. Using a sep funnel I separated the two layers keeping each. After I cleaned up and put away the expensive stuff I took a couple of ml of the dark yellow solution and lit it with a match attached to a stick while standing behind a tree (still had the safety shield on). It burned and fizzed and got quite hot. No explosion.

Now a new question, I should have all three isomers of nitrotoluene, para, meta, and ortho. I'd like to somehow separate the ortho from the others and can't find any method to accomplish this. The physical data indicates that the para should crystalize (melting point 54.5C) it didn't. I took the temperature down to -10C, no crystals, no freezing, nothing...

Any suggestions??


Rhodium
Administrator   posted 07-01-98 04:33 AM          
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You have as good as no meta-nitro isomer. The other two isomers are pretty hard to separate, but if you first reduce your nitrotoluene to a mixture of o- and p-toluidine, the isomers are easier to separate.
After you have reduced the nitrotoluenes, and steam distilled them together, pour off the water, and chill the toluidine mixture through adding ice and salt. A whitish-yellow crystalline mass precipitates, which is the hydrate of p-toluidine. This is filtered off at the pump in a chilled buchner funnel, and is well pressed to remove any oily o-toluidine. The o-toluidine is separated from the salt/water with a sep funnel. The purification can be repeated if desired. Finally, dry the pure o-toluidine.


Cheapskate
Member   posted 07-01-98 09:44 AM          
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Rhodium, your FAQ indicates I can reduce the NT to toluidine using Fe or Sn CZ_74 suggested SnCl2/HCl. I can get this, but it's about two weeks away. How about disolving iron oxide in HCL. I have the iron oxide from thermite experiments and can try that easily. I'd just rather not waste the NT if there's no hope of it working.
 
Rhodium
Administrator   posted 07-01-98 09:47 AM          
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No, your ordinary red iron oxide won't do, it is already as oxidized as it can be, and it can therefore not reduce the nitro groups.
 
Cheapskate
Member   posted 07-01-98 10:19 AM          
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OK, I'll have to place the order and wait. I guess I'll start on other phases of the project. Thanks for your help, I'll be bothering you more in the future.
 
mcdowell
unregistered   posted 07-02-98 06:56 PM           
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Rhodium is there hypotheticaly any way of speeding up the first part of the manas A using a microwave oven?
 
Rhodium
Administrator   posted 07-02-98 09:41 PM          
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You tell me. I have not the slightest idea about how the microwaves interacts with the different reactions that goes well with the aid of it.
The reaction of isatoic anhydride with o-Toluidine is a simple reaction, go see if someone else has made amides from anilines and anhydrides with good results with MW.


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