Melgar
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Isopropylamine via sulfuric acid, propylene (MAPP PRO gas), and sulfamic acid?
This patent got me thinking about an easy synthesis of isopropylamine:
https://www.google.com/patents/US2504807
Sulfuric acid with P2O5 added to it until it started to fume should work fine, I imagine, and MAPP PRO gas is just propylene and propane mixed, if I
remember right. I am 100% sure that there's substantial amounts of propylene in it and that it's the main, if not only alkene.
For the ammonia, it'd probably be easier to add sulfamic acid instead of setting up an anhydrous ammonia gasser. Since at 100% sulfuric acid, you
have small quantities of SO3 in the mix at all times, and sulfamic acid is basically an adduct of ammonia and SO3, it should be fairly
straightforward, no?
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Corrosive Joeseph
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Quote: Originally posted by Melgar  | and MAPP PRO gas is just propylene and propane mixed, if I remember right. I am 100% sure that there's substantial amounts of propylene in it and
that it's the main, if not only alkene.
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Confirmation -
"MAPP gas" - https://en.wikipedia.org/wiki/MAPP_gas
"MAPP gas" is a trademarked name, belonging to The Linde Group, and previously belonging to the Dow Chemical Company, for a fuel gas based on a
stabilized mixture of methylacetylene (propyne) and propadiene.
The name comes from the original chemical composition, methylacetylene-propadiene propane.
"MAPP gas" is also widely used as a generic name for UN 1060 stabilised methylacetylene-propadiene (unstabilised methylacetylene-propadiene is known
as MAPD).
MAPP gas is widely regarded as a safer and easier-to-use substitute for acetylene.
In the spring of 2008, true MAPP gas production ended in North America when production was discontinued at the only remaining plant in North America
that still manufactured it.
Current products labeled "MAPP" are, in fact, MAPP substitutes. These versions are stabilized liquefied petroleum gas (LPG) with high levels of
propylene.[1]"
VERY interesting............. P2O5 is a problem for me. Is there anyway around it..............?
/CJ
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Melgar
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| Quote: Originally posted by Corrosive Joeseph | Current products labeled "MAPP" are, in fact, MAPP substitutes. These versions are stabilized liquefied petroleum gas (LPG) with high levels of
propylene.[1]"
VERY interesting............. P2O5 is a problem for me. Is there anyway around it..............?
/CJ |
SO3? But that doesn't seem nice at all.
If you can get red phosphorus and burn it inside a flask though, it'll coat the inside with thick, white fluffy P2O5. Much more P2O5 than starting
phosphorus, too. And if you use that flask for your reaction next, there's no need to even scrape the white stuff out. Really, you just need fuming
sulfuric acid, meaning there's a small amount as SO3 at any given time. There are probably quite a few ways of getting fuming sulfuric acid written
on these boards. Even just boiling regular 96%+ sulfuric acid might work, although I can't imagine that's pleasant to work with.
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UC235
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Considering most glyphosate herbicide is sold as the isopropylamine salt from which it is readily liberated by NaOH, this seems extremely superfluous
and dangerous. In fact, nothing about using P2O5, SO3, or MAPP gas seems "easy."
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Melgar
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P2O5 is just an extremely hygroscopic white powder that quickly forms a gooey polyphosphoric acid coating over it that prevents it from reacting very
quickly at all. SO3 would only be formed in very small quantities, virtually all of which would stay in solution. And there isn't any oxidizer or
pyrophoric chemical around. Obviously the propane bubbles would need to be properly vented though. The main thing to watch out for would probably be
brown, polymerized crap, which now that I think about it probably means decanting the sulfuric acid from the P2O5, which has by now formed a gooey
slime all over the inside that isn't going anywhere even if you wanted it to. (An overnight soak in water will remove it entirely though)
I could do this in 10-15 minutes, since I have a bottle of sulfuric acid, a tub of P2O5, and I could tape up the air holes on my shittier torch and
run the gas with a tube into the mixture. Cleaning up, on the other hand, I don't foresee as being fun at all, which is why I hesitated to do it.
Also, I don't have good enough ventilation for the aforementioned propane gas and its odorant.
Good to know about the glyphosate salt though! I did an SDS check of nearby places and even though most of the herbicide is like 2% active, there are
a few concentrated ones that are like 18%. So maybe 5% isopropylamine? It comes out to about $20 for 50 mL, assuming perfect yields. I could buy it
more concentrated, but then I'd have to get it in the 1-gallon or 2.5-gallon sizes. Might also be good to see if there's anything else useful in it.
My Whole-Foods-patronizing, anti-GMO roommate would have a seizure if he saw me distilling glyphosate though. 
My dad is a farmer though, and he may have some extra laying around, but I'd have to make sure it was the isopropylamine salt, plan a trip upstate,
etc.
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Corrosive Joeseph
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A popular glyphosate herbicide in my area has this printed on the front label -
"This product is a soluble concentrate containing 360g/l (30.77% w/w) glyphosate, present as 480g/l (41.6% w/w) of the isopropylamine salt of
glyphosate"............ Does that mean there is 120g of IPA in a one litre bottle then............?
This seems to be a fairly standardized strength of it. It is quite expensive by the half litre here (€15), I'm sure it's cheaper by the 20 litre
cans and it's used on farms all over the world all the time..........
Is there really a need for the P2O5...............? It is unobtainium for me........... But..........
Taken from the linked patent above -
"A di-isopropyl sulfate liquor may be prepared by gassing -l00% strength sulfuric acid with sufficient propylene to react with substantially all the
acid to thereby form predominantly isopropyl sulfate.
For example, gassing of the sulfuric acid with propylene is preferably effected at temperatures in the range of zero to minus 10 (3., and when
utilizing 95-100% strength sulfuric acid about 2 mols of propylene are needed for each mol of H2504."
Looks like 95% H2SO4 works...........
/CJ
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Melgar
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Sulfuric acid can actually go above 100%, the way its percentage is given. When there is SO3 present, that counts as "negative water" and thus above
100% H2SO4. At or very close to 100%, there is roughly as much free SO3 as free H2O; very little of either, but enough for a reaction to take place
at a steady rate. Drop a percentage or two lower though, and no reaction.
I brought up P2O5 because it's the one thing I have that can pull water from sulfuric acid, but that might not even work without distillation (it
could react with the propylene somehow), and I'm sure there are other ways. The important thing is finding a way to get sulfuric acid to where H2O
and SO3 are in approximate equilibrium. Since patents often give much wider ranges than actually work to throw off people trying to copy them, and
since you never know the concentration of the drain opener stuff anyway, it's probably good to fortify it somehow. I'm not aware of any stronger
desiccants that a home chemist could obtain than P2O5 (that are also non-reducing), so instead of removing water, the other option is to add SO3. Of
course, you might get lucky and have it work at 95% too.
Your calculation for the mass per liter seems about right, since it correlates with what I figured. I wonder if ion exchange resins could separate
this stuff out from the rest of it? Seems like they'd be the only significant anions.
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Corrosive Joeseph
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Check page 2 of this thread for posts by Scr0t and Magpie - http://www.sciencemadness.org/talk/viewthread.php?tid=14442&...
/CJ
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JJay
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I wonder if you could distill isopropylamine from sodium amide and potassium isopropyl sulfate.
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Melgar
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Sodium amide with isopropyl sulfate!? At least you wouldn't have to worry about your heat source, since the reaction would provide MORE than enough
heat on its own!
As for the second page, the Leuckart reaction won't work because of the special reaction between acetone and ammonia, that gives triacetoneamine.
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JJay
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Actually, I am pretty sure you would have to heat it; isopropyl sulfate and alkali isopropyl sulfates have very different properties. It's like
comparing hydrogen chloride and table salt.
Edit: Perhaps I misunderstood... if you meant sodium amide and isopropyl sulfate, as in isopropyl sulfuric acid.... I don't think that would work very
well, although it might possibly produce some of the desired product with a large excess of sodium amide. Even that would likely require heating due
to the large amount of ammonia gas being given off with its high heat of vaporization. If you meant diisopropyl sulfate... that would probably work
without any heating, at least for the first half of the reaction. I'm thinking you'd probably want slow addition with high dilution to avoid an out of
control exothermic reaction, but it could be tricky to avoid getting a mixture of products.
[Edited on 4-7-2017 by JJay]
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Melgar
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I would think that somehow the sulfate would be reduced, since even iron and zinc can reduce sulfates, or there would be a condensation reaction
between sodamide and sulfate or something; there just seem to be a lot of potential routes for it to blow up on you. It's like mixing sulfuric acid
and lithium aluminum hydride or something, it just seems like a bad idea, but you can't exactly say why.
To be fair I once tried mixing tiny quantities of LiAlH4 and H2SO4 once to see what it would do, and it just bubbled slowly, so my instincts on these
things are often wrong. Adding a drop of water to this, on the other hand, made it blow up in a near-detonation, shattering the test tube.
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