gluon47
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Methyldichloramine
I have been trying to make some Methyldichloramine.
Apparently it can be made by the action of hypochlorous acid on methylamine salts
I did a few tests to see how easy this was:
1. I added some methylamine hydrochloride to a beaker. To this I added some 4% sodium hypochlorite bleach. There was a lot of fizzing (A reaction
seemed to occur). I added some 5% acetic acid to convert the sodium hypochlorite to hypochlorous acid.
A separate layer formed on the top of the mixture. I presumed this was the methyldichloramine. After a few minutes the layers had began to merge and
soon the mixture was homogenous.
I've tried this 3 times and had the same result.
How can I extract the methyldichloramine from this mix?
I don't want to try distilling it out because I've heard it explodes when heated with water.
Should I just collect the top layer before it merges. Is this the methyldichloramine?
Would a non-polar solvent (like toluene) be capable of extracting the methyldichloramine?
Presumably the methyldichloramine could then be distilled off without the risk of explosion?
Any help appreciated.
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PHILOU Zrealone
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Way to dilluted reactants...
There is a tread by Axt in the energetic material section about chloramines and haloamines.
Those are sensitive powerful explosives said to be as potent as nitroglycerin.
Extraction with a solvent may work if the solvent is unreactive towards it...but CH3-NCl2 is likely a source of Cl(+) and it will probably chlorinate
toluen forming CH3-NH2 back...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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gluon47
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Thanks for the response!
I didn't know the methyldichloramine and chloramines in general were particularly explosive.
I just want to make an alkyldichloramine and the only alkylamines I have are isopropylamine and methylamine.
Axt made isopropyldichloramine in the thread you referred to. I tried to replicate his procedure but I coulden't get it to work.
I did this over a year ago so I cant remember all the quantities
I added 47g of isopropylamine.HCl to 500ml (I think) of 5% bleach. I chilled this mixture down to about 0 C and added 33% hydrochloric acid (can't
remember how much) slowly over the course of several hours. I stirred the mixture for 10 minutes by hand.
axt reported that the isopropyldichloramine separated at this point as a yellow oil. this did not happen for me. I left the mixture overnight and in
the morning there was still no layer .
despite this, perhaps isopropyldichloramine would be a more realistic target as it doesn't need to be extracted with a solvent.
Does anyone know were could I have gone wrong? any obvious mistakes?
[Edited on 4-6-2016 by gluon47]
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PHILOU Zrealone
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Maybe too diluted bleach (5% is weak)...you could get 10-15-25% for Professional cleaning.
I would use concentrated acetic acid not HCl...because you want HOCl not Cl2(gas) nor Cl2O (gas)...
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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gluon47
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Of course! I forgot HCl and NaOCl produce chlorine.
I do have access to glacial acetic acid and I could probably make some concentrated bleach just like axt did
from Cl2 and NaOH. Or maybe buy some from a cleaning store as you suggested.
I'll retry the synthesis soon using conc bleach and glacial acetic acid.
I'm currently out of isopopylamine so I'll have to extract some from roundup first.
thanks for your help
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CuReUS
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there are other ways to make the target compound
1. using TCCA - http://www.sciencemadness.org/talk/files.php?pid=69963&a...
2.using NCS - https://www.thieme-connect.com/products/ejournals/abstract/1...
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gluon47
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fascinating! I can get hold of trichloroisocyanuric acid.
I'll have to try this method as well. thanks for sharing
N-chlorosuccinimide might be a bit harder.
I finally feel like I might be close to preparing an alkyldichloramine!
[Edited on 5-6-2016 by gluon47]
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aga
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methyl dichloramine or isopropyl dichloramine ?
Are 'methyl' and 'isopropyl' the same thing ?
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gluon47
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Quote: Originally posted by aga  | methyl dichloramine or isopropyl dichloramine ?
Are 'methyl' and 'isopropyl' the same thing ?
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No. I initially wanted to synthesize methyldichloramine, but I realized isopropyldichloramine would probably be eaiser and safer.
so I changed my target compound to isopropyldichloramine.
CH3-NCl2 = Methyldichloramine
CH3-CH2(NCl2)-CH3 = Isopropyldichloramine
Methyl and isopropyl radicals are not the same.
[Edited on 5-6-2016 by gluon47]
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Polysialate
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It's worth noting that solid calcium hypochlorite can be acquired easily/cheaply for pool chlorination.
Alternatively, I think bleach by concentrated to a ~pentahydrate by storing in a sealed container with some desiccant. Will take some time and a lot
of desiccant, though.
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PHILOU Zrealone
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| Quote: Originally posted by gluon47 |
CH3-NCl2 = Methyldichloramine
CH3-CH2(NCl2)-CH3 = Isopropyldichloramine
Methyl and isopropyl radicals are not the same.
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Isopropyl radical is CH3-CH(-)-CH3 or (CH3)2CH-
You have a H atom too much...
This looks familiar to me....reminds me the mistakes of a banned multiple ID poster (octonitrocubane, A nitrogen rich explosive, Eosin Y, Eosin Y
again, ...) 
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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gluon47
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Your right, Sorry I'm no master of organic chemistry.
I swear I'm not any of the above. I just like making obscure compounds.
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