| Pages:
1
2 |
Agent MadHatter
Harmless
Posts: 45
Registered: 22-7-2009
Member Is Offline
Mood: No Mood
|
|
Storing Diethylamine?
I recently distilled over 100grams of Diethylamine, but I can't find any information on storing it. I don't believe it reacts with light, but I don't
want it to decompose either.
What is the best way to store decent sized amounts?
|
|
|
kclo4
National Hazard
Posts: 916
Registered: 11-12-2004
Location:
Member Is Offline
Mood: No Mood
|
|
Are you sure it is diethylamine?
It might be good to keep it in a salt form.. such as its hydrogen chloride or sulfate.
I'd store it in a cool dark place in a glass container..
|
|
|
Agent MadHatter
Harmless
Posts: 45
Registered: 22-7-2009
Member Is Offline
Mood: No Mood
|
|
Its in HCL form, and its in a flask with a stopper on it at the moment. Positive its Diethylamine.
|
|
|
zed
International Hazard
Posts: 2283
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
Exclude air. Brown glass bottle. Cool dark place.
|
|
|
entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
Member Is Offline
Mood: Fissile
|
|
Anyone else find it odd that he's positive what he's got but hasn't a clue how to store it??
|
|
|
kclo4
National Hazard
Posts: 916
Registered: 11-12-2004
Location:
Member Is Offline
Mood: No Mood
|
|
How did you get it? DEET hydrolysis?
You ought to report the success, not many people know if it works well or not.
|
|
|
Agent MadHatter
Harmless
Posts: 45
Registered: 22-7-2009
Member Is Offline
Mood: No Mood
|
|
Hows it odd? I'm positive I have it, because I took off the acid and made it freebase and watched my product disappear into the air.
I did do hydrolysis though...I don't feel like I'm the right type of candidate to make a report about it.
|
|
|
kclo4
National Hazard
Posts: 916
Registered: 11-12-2004
Location:
Member Is Offline
Mood: No Mood
|
|
| Quote: |
I did do hydrolysis though...I don't feel like I'm the right type of candidate to make a report about it. |
I'd still report back the success you've had, how you did it, some simple observations, etc... That would at least be giving back to the community
that has helped you out a lot with this little project..
|
|
|
entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
Member Is Offline
Mood: Fissile
|
|
Well that proves it for sure!
No point in messing around with the Hinsberg test and other silliness, is there?
|
|
|
Agent MadHatter
Harmless
Posts: 45
Registered: 22-7-2009
Member Is Offline
Mood: No Mood
|
|
Eh. I don't know how to do a Hinsberg test...
But I'll report back. Whats your name on TV?
|
|
|
kclo4
National Hazard
Posts: 916
Registered: 11-12-2004
Location:
Member Is Offline
Mood: No Mood
|
|
Well, what other compound would form from H2SO4 or HCl and DEET? assuming that is how you made it..
|
|
|
Agent MadHatter
Harmless
Posts: 45
Registered: 22-7-2009
Member Is Offline
Mood: No Mood
|
|
After hydrolysis I believe toluic acid would be left with Diethylamine. I distilled the DEA in a container with some HCL in it.
|
|
|
entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
Member Is Offline
Mood: Fissile
|
|
What else could it be? Who could even guess? He's not telling us how he thinks he made it. I guess he will divulge details after he gets a patent.
I think the claim of 100 gms of DEA is suspect if we're talking about the hydrolysis of DEET.
|
|
|
DJF90
International Hazard
Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline
Mood: No Mood
|
|
I'm with entropy; to make 100g Et2NH2Cl you require a yield of 100% on the hydrolysis of 176.3g DEET. Thats in excess of £17
(retails at about £10/100mls). Now factor in that the yield will not be 100% (probably more likely to be between 60 and 90%, depending on conditions
etc) and its looking expensive, especially for less than a mole of reagent.
Also with the acid hydrolysis of DEET you will not distil the diethylamine from the reaction mixture...
[Edited on 15-9-2009 by DJF90]
|
|
|
Picric-A
National Hazard
Posts: 796
Registered: 1-5-2008
Location: England
Member Is Offline
Mood: Fuming
|
|
Just a quick note, 100% deet can be had for half the rrp off ebay UK
If this guy thinks hes distilling DEA.HCl from the mix he should really learn some basic chemistry
[Edited on 15-9-2009 by Picric-A]
|
|
|
entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
Member Is Offline
Mood: Fissile
|
|
I was giving him the benefit of a doubt that he either (a) hydrolyzed in base, in which case the DEA could be distilled out, or (b) hydrolyzed in
acid, then added base.
I'm thinking he meant he distilled it INTO HCl. But that wouldn't form the crystals of the amine HCl that he seems to think he has, would it? No
mention of using HCl in Et2O, which would form crystals.
I love chemical mysteries!
We'll be able to figure it all out when his patent is issued.
[Edited on 15-9-2009 by entropy51]
|
|
|
Picric-A
National Hazard
Posts: 796
Registered: 1-5-2008
Location: England
Member Is Offline
Mood: Fuming
|
|
I think he distilled the amine out into HCl(aq) then boiled down forming the salt!
but indeed this is a mystery, no wonder he doesnt want to document it
[Edited on 15-9-2009 by Picric-A]
|
|
|
DJF90
International Hazard
Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by Picric-A  |
If this guy thinks hes distilling DEA.HCl from the mix he should really learn some basic chemistry
[Edited on 15-9-2009 by Picric-A] |
I seem to recall you making the same mistake (not basifying) here: http://www.sciencemadness.org/talk/viewthread.php?tid=12366#...
And as to the mystery, we're still waiting on pictures of that contact process plant. I wander why you dont want to document it...
|
|
|
panziandi
Hazard to Others
Posts: 490
Registered: 3-10-2006
Location: UK
Member Is Offline
Mood: Bored
|
|
I suspect it was base hydrolysis with vapours leading over to hydrochloric acid,which was evaporated down and crystalised and stored? I suspect this
was the route chosen, however, DEA.HCl will be very hygroscopic and deliquescent, probably difficult to crystalise nicely. I would personally store
it, assuming it is the chloride, as the solid in an amber glass jar with a tight fitting wadded lid preferably in a dessicator over solid sodium
hydroxide, as one should store methylammonium and ethylammonium chlorides. Alternatively if it is the free amine, a brown glass bottle with a polycone
style lid would be suitable.
Oh dear, caught out? I expect Picric-A learnt from his mistake? I mean he is going to try the infamous Skraup reaction, notorious for run aways,
remember the quinoline is an amine so don't try and distil any quinoline.H2SO4 
[Edited on 15-9-2009 by panziandi]
|
|
|
DJF90
International Hazard
Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline
Mood: No Mood
|
|
It is possible base hydrolysis was used, although the thread author says he expects (m-)toluic acid to remain in the flask. So he could have
done it either way. But in any case there seems to be a fundamental misunderstanding of acid-base chemistry (and he isnt the only one  ); you cant have toluic acid after a basic hydrolysis, and you cant distill
diethylamine after an acid hydrolysis, unless of course he basified and forgot to mention it...
|
|
|
Picric-A
National Hazard
Posts: 796
Registered: 1-5-2008
Location: England
Member Is Offline
Mood: Fuming
|
|
Yes so i then went out and learnt the basic chemistry- im not being a hypocrite!
I cant no be bothered to repeat what i have said so many times before
|
|
|
panziandi
Hazard to Others
Posts: 490
Registered: 3-10-2006
Location: UK
Member Is Offline
Mood: Bored
|
|
So I would quite like to know how the thread's author actually went about this. Because the DEA thread has kind of been a drag to keep up with over
the months, in fact I gave up on it until recently something caught me eye again but I quickly gave up. Would be nice to see someones detailed attempt
at this, method, yield pictures perhaps?
|
|
|
sonogashira
National Hazard
Posts: 555
Registered: 10-9-2006
Member Is Offline
Mood: No Mood
|
|
Here is some information on purification from Armarego:
Diethylamine [109-89-71 M 73.1, b 55S0, d 0.707, n 1.38637, pK15 11.38. Dried with LiAlH4
or KOH pellets. Refluxed with, and distd from, BaO or KOH. Converted to the p-toluenesulfonamide and
crystd to constant melting point from dry pet ether (b 90-120°), then hydrolysed with HCl, excess NaOH was
added, and the amine passed through a tower of activated alumina, redistd and dried with activated alumina before
use [Swift JAm Chem Suc 64 115 19421.
8 A polystyrene diethylaminomethyl supported version is commercially available.
Diethylamine hydrochloride [660-68-41 M 109.6, m 223.5O. Crystd from absolute EtOH. Also
crystd from dichloroethane/MeOH. Hygroscopic.
|
|
|
kclo4
National Hazard
Posts: 916
Registered: 11-12-2004
Location:
Member Is Offline
Mood: No Mood
|
|
Be interesting to see at least a write up, etc.
|
|
|
sonogashira
National Hazard
Posts: 555
Registered: 10-9-2006
Member Is Offline
Mood: No Mood
|
|
What is to write up?! It is a hydrolysis!
|
|
|
| Pages:
1
2 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
