1911
Harmless
Posts: 13
Registered: 29-6-2011
Location: Finland
Member Is Offline
Mood: No Mood
|
|
Preparation of trimethyl phosphate
Here is the procedure I've been thinking:
93ml phosphoryl chloride was slowly added to 40ml methanol containing 139ml triethylamine under constant stirring.
The step that bothers me is how I should remove triethylamine hydrochloride from TMP. Are there any other means besides distillation at lowered
pressure to get rid of the salt. I do have a rotary vacuum pump but I'm not very experienced with low pressure distillations so I would preferrably
use some other way particularly with carcinogenic methylating agents.
|
|
|
Endimion17
International Hazard
Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline
Mood: speeding through time at the rate of 1 second per second
|
|
There's a whole subsection of SM dedicated to organic chemistry, check it out.
|
|
|
1911
Harmless
Posts: 13
Registered: 29-6-2011
Location: Finland
Member Is Offline
Mood: No Mood
|
|
Well actually I wasn't quite sure if this was organic or non-organic chemistry as TMP is a ester of a non-organic acid so I decided to go with
Chemistry in general. But yes this might belong to organics when I think about it...
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I do not think any of you should help contribute to this thread,
the same synthesis used to make trimethyl phosphate could also be used on fluorophosphate, which is readily obtainable, to make methyl fluorophospate
esters, which is essentially nerve gas.
[Edited on 25-3-2012 by AndersHoveland]
|
|
|
AJKOER
Radically Dubious
Posts: 3026
Registered: 7-5-2011
Member Is Offline
Mood: No Mood
|
|
Thanks AndersHoveland.
I decided to remove my suggestions (deleted respond).
|
|
|
Endimion17
International Hazard
Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline
Mood: speeding through time at the rate of 1 second per second
|
|
But the thread about making fucking amphetamines is ok?
http://www.sciencemadness.org/talk/viewthread.php?tid=6380
|
|
|
BromicAcid
International Hazard
Posts: 3245
Registered: 13-7-2003
Location: Wisconsin
Member Is Offline
Mood: Rock n' Roll
|
|
Trimethyl phosphate is not the methylating agent that say dimethyl sulfate is. Usually more driving conditions are used. Distillation may be your
best bet, just flash it over, at atmospheric the boiling point is still <200°C, not bad at all for a phosphate ester. Still, I wouldn't rule out
entraining some triethylamine salts and bringing them over as well.
You could always try to find a solvent in which your trimethyl phosphate is soluble that is fairly non-polar which could crash out your impurities and
then flash off that second solvent at a lower temp.
|
|
|
1911
Harmless
Posts: 13
Registered: 29-6-2011
Location: Finland
Member Is Offline
Mood: No Mood
|
|
Thank you Bromic. My intentions are not in nerve gases but in methylations of certain phenolic compounds in which trimethyl phosphate works as stated
in this patent http://www.freepatentsonline.com/4453017.html
I think that when I get an aspirator pump I could even try the vacuum distillation. I definitely won't be happy to distill that at 195 deg. C. About
that solvent I would think diethyl ether might do. But is triethylamine hydrochloride soluble in trimethyl phosphate anyways?
|
|
|
woelen
Super Administrator
Posts: 8012
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
@AndersHoveland: If your argument was valid, then we should not have sciencemadness at all. Any synthesis method can be used to make nasty compounds.
The methyl phosphate esters are not the bad compounds you are referring to. Only if someone directly asks for synthesis of nerve agents (or drugs, or
whatever dangerous/toxic/illegal compound) then it is time to frown upon it.
|
|
|
neptunium
National Hazard
Posts: 989
Registered: 12-12-2011
Location: between Uranium and Plutonium
Member Is Offline
|
|
he said he is not experienced with vacuum distillation chances are he cannot (probably would not) take a chance with nerve gas and highly confined
airtight clean box with electronic monitoring. and if he does he will never reply to tell you it worked.
|
|
|
mnick12
Hazard to Others
Posts: 404
Registered: 30-12-2009
Location: In the lab w/ Dr. Evil
Member Is Offline
Mood: devious
|
|
From my own expirience I can say that TMP is a decent methylating agent. It is capable of methylating most phenolic aldehydes (had bad results with
5-methoxysalicylaldehyde), and can even be used in the permethylation of hydroquinone. However the main drawbacks are longer reaction times, harsher
conditions, and a cruder product.
Unless it is unavailable, I would suggest you simply purchase the material rather than synthesize it.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
