02-09-04 12:01
No 487507
I came across some information yesterday whilst I was reading, and the material I was reading sugeested that nitromethane could be synthesized from methyl sulfate and sodium nitrate. I can't vouch for the validity of this information, and from what I saw in other parts of the material, I'd tend to doubt it. But I'm still intrigued as to whether or not it is possible. My thoughts were that it was a typo, and it should have read sodium nitrite, which I know will not form nitromethane, it will only form methyl nitrite. So what are bee's thoughts on this, is the info way off?
It is seductive, way too seductive. -Eleusis
(Newbee)
02-09-04 13:24
No 487515
The nitrate wont form aliphatic nitro compounds. Only nitrate-esters w/ alcoholes (esterification w/ nitric acid) eg. methyl nitrate, nitroglycerin, etc. Or nitrate aromatic rings (electrophyl subst.) eg. nitrobensol, etc.
With nitrite you could form the desired aliphatic nitro compounds, the way you want.
Even w/ alkai salts of monoalkylsulfuric esters (NaMeSO4, NaEtSO4)
:Post 251119 (Bandil: "Nitroethane ala Antoncho succes", Novel Discourse)
Post 233762 (Antoncho: "Kitchen nitroalkane success!", Chemistry Discourse)
" Unorthodox cooking, illicit cooking. A bit of real science, in fact. "
(Hive Addict)
02-16-04 14:43
No 489149
FIELD: industrial organic synthesis. SUBSTANCE: method of producing nitromethane from sodium nitrate and methyl esters in an aqueous medium is distinguished by that those methyl esters (methylation agents) are dimethyl oxalate, dimethyl sulfate, trimethyl phosphate, methyl thiocyanate, methyl tosylate, methyl benzenesulfonate. EFFECT: enlarged choice of raw materials.
Patent RU2138478
If only Biodiesel could be used as a methyl ester
(Hive Addict)
02-16-04 17:09
No 489178
A kind russian bee has confirmed that these people are illiterate... Post 489172 (dennis_pro: ":( It is very brief patent", Russian HyperLab)
Ohwell.. That was starting to look cool.. Sulphuric aicd, (m)ethanol, and OTC alkali nitrate-> EtNO2 & MeNO2
(Stranger)
02-16-04 19:33
No 489204
just heat the nitrate to form the nitrite first.
(Hive Addict)
02-16-04 19:47
No 489206
Have any details?????????? You shuld know by now that insignificant postings are not allowed boy! Elaborate and share this wonderful info
I have yet to see a pratical method for making nitrite!
I remember reading an inconclusive report of making teeny ammounts on the explosives forum which was not pure enough, having mixtures of two, three, and even four salts.
Besides as denis_pro states, it does not contain any reaction details. So the alkylester & alkali nitrite route would require some experimentation. I think it looks alot easier and less time consuming than the alakli alkylsulfate, possibly having higher yields.
(Stranger)
02-16-04 22:43
No 489247
ive been looking in TFSE and the reaction of the bees is negative. they say C and alkali nitrate explode on heating. they say on heating alone they end up with the oxide. and they are 100% correct.
it is a matter of technique. yes, the refs give dec of nitrite at its mp, im sure it does. but if done right you can get a decent yield w/o resorting to making nitrite from HNO3, also an option.
for the Pb reduction mentioned elsewhere, the temp is 400-450C. this means stirring is a must. the Pb is melted 1st!
for C: dont heat it so hard and it wont explode! even so, this risk is not worth taking.
i wonder if people are using a very hot direct heat on their failed attempts to make nitrite. i know that careful heating to the mp and visually looking at the reaction help. if at first...give up? of course they dried 1st.
i am unfamiliar with the sodium salt, but the KNO3 is widely sold here and i know that if dried then heated to 425C in a stainless crucible-gently- then quickly cooled a product is formed that gives all the reactions of nitrite.
so its not pure, i know, the Pb method is better for that, and so is reduction of HNO3. but the characteristic cpds from the nitrite have been prepared in acceptable yield easily separated by dist and redist.
also, you dont need C or C and S to make nitrate explode. it will do this on its own if you use a strong heat.
a method i havent tried- H2 and molten nitrate. no gentle bubbling here, its gotta be fast.
the reduction of acid was done long ago in school. hot acid, Cu, hot carbonate soln, blah blah. works but is wasteful of acid.
there is no simple answer
(get it?)
(Official Hive Translator)
02-17-04 00:21
No 489258
..has been posted in Post 489255 (Antoncho: "Not quite....", Russian HyperLab)
It contains useful details on making nitromethane from other methylating agents (methyl tosylate, dimethyl sulfite etc) and NaNO2.
Antoncho
(Moderator)
03-23-04 17:37
No 496937
(Rated as: excellent)
The following article by Desseigne and Giral, from Memorial des Poudres, 34, 13-53 (1952) as requested in Post 495484 (moo: "Nitroethane", Methods Discourse) should bee quite helpful to those attempting this synthesis
Despite the imperfections, this was the best that could bee done under the circumstances 
Chemistry is our Covalent Bond