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Melgar
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Quote: Originally posted by JJay  | | 30% hydrogen peroxide. I am about to lose my pirannah virginity. I guess it's like getting married? |
Base piranha is underrated, in my opinion. It evaporates if you accidentally spill a few drops of it and if you get it on your skin, it stings, but
probably less than 30% H2O2 by itself. It also leaves the white peroxide marks for a few minutes. Reason being, base piranha needs to be around the
H2O2 thermal decomposition temperature to work. The ammonia seems to have the effect of reducing the likelihood of thermal runaway though, as opposed
to acid piranha that has been known to explode, and can transition to thermal runaway very quickly.
Maybe try for third base before losing it? 
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JJay
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No, I'm going all the way  I have a really filthy Graham condenser that I'd
prefer not to have to replace. Cleaning it calls for extreme measures. If piranha doesn't work, I'll be posting pictures of my new Graham condenser
pretty soon.
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tsathoggua1
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2kg phosphorus (red)
100g cinnamyl chloride
100ml n-butyric anhydride
20g Li metal, or may have been 25g
500g iodine
5g 3-fluoro-4-(1,1-difluoromethoxy)-5-methoxybenzaldehyde
250g n-dodecanethiol
500ml SOCl2
1l nitroethane
Couple of welding-size argon cylinders and 1 of CO2
2l 98% H2SO4
(unsure of the weight, came from a pet store) bottle of methylene blue solution)
500ml conc. HCOOH
And not bought, but a script from my dr. for KMnO4. Needed a portion of one tablet for my foot, to bathe it in, but given a few pots. I am not going
to turn that down. In fact I'm going to shoot for getting it on repeat
Not too familiar with base piranha, never used it. But with the acid version make sure there are no organics left. It'll oxidize inorganic carbon to
CO2 and there is the potential (probability?) for anything but the tiniest traces of organics to result in a nasty explosion. Not a pretty thing to be
covered by conc. H2SO4 and H2O2
[Edited on 9-2-2017 by tsathoggua1]
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Db33
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I was at ACE hardware looking around because they are the only store in the area that has Toluene. While i was there i also got pure Citric Acid and
noticed that they sell pure ethyl Acetate. Im considering buying it. its about $9 per Liter. I dont have a specific use for it but from what i recall
its a very useful chemical to have.
For those that are interested its actually in the paint thinner section its called Klean Strip M.E.K. Substitute.
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Geocachmaster
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@Db33 I thought that Klean Strip M.E.K. substitute wasn't sold anymore. In fact, Klean Strip's website has it on the discontinued page, as the 12th item. I checked Ace's website as well and I could not find it there either. Did they just start selling it again?
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JJay
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I had thought they banned ethyl acetate for sale in some states (for reasons that I don't claim to know or understand)... I do know that I've seen
Rust Remover, Rust Converter and TSP Substitute on shelves recently. I'm guessing that these are products that don't sell very well, and for that
reason, a lot of places still have stocks of them.
I distilled some ethyl acetate from nail polish remover one time, but I think some additional purification steps were required... I don't remember
offhand.
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gdflp
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| Quote: Originally posted by JJay | I had thought they banned ethyl acetate for sale in some states (for reasons that I don't claim to know or understand)... I do know that I've seen
Rust Remover, Rust Converter and TSP Substitute on shelves recently. I'm guessing that these are products that don't sell very well, and for that
reason, a lot of places still have stocks of them.
I distilled some ethyl acetate from nail polish remover one time, but I think some additional purification steps were required... I don't remember
offhand. |
I believe that it was actually due to MEK getting banned from commercial use a while ago. When
the regulations on MEK got eased recently, Kleen Strip stopped manufacturing the MEK substitute. Probably either because MEK is cheaper than EtOAc or
MEK is the superior solvent in the intended use(or both, I'm not sure). I saw a good 20 1L cans of MEK substitute sitting on the shelf at my local
ACE a couple days ago, so they must still have pretty good stock on it though.
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JJay
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That makes sense... I usually just buy acetone and have never actually used MEK for anything, so IDK.
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Cryolite.
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| Quote: Originally posted by tsathoggua1 | 2kg phosphorus (red)
100g cinnamyl chloride
100ml n-butyric anhydride
20g Li metal, or may have been 25g
500g iodine
5g 3-fluoro-4-(1,1-difluoromethoxy)-5-methoxybenzaldehyde
250g n-dodecanethiol
500ml SOCl2
1l nitroethane
Couple of welding-size argon cylinders and 1 of CO2
2l 98% H2SO4
(unsure of the weight, came from a pet store) bottle of methylene blue solution)
500ml conc. HCOOH
And not bought, but a script from my dr. for KMnO4. Needed a portion of one tablet for my foot, to bathe it in, but given a few pots. I am not going
to turn that down. In fact I'm going to shoot for getting it on repeat
Not too familiar with base piranha, never used it. But with the acid version make sure there are no organics left. It'll oxidize inorganic carbon to
CO2 and there is the potential (probability?) for anything but the tiniest traces of organics to result in a nasty explosion. Not a pretty thing to be
covered by conc. H2SO4 and H2O2
[Edited on 9-2-2017 by tsathoggua1] |
Where do you drug chemists get such quantities of phosphorus and nitroethane?
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Db33
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ill take a photo of it, its still on the shelves here but youre right, it does appear to be being replaced by the old MEK. i might as well get a few
bottles while its still here!
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Db33
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actually i went back today and now they only had 1 bottle left and i got it, so it seems as though it might be just them clearing out there inventory.
So if you need some or just want some pure ethyl acetate id get some before its gone.
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JJay
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| Quote: Originally posted by Cryolite. | | Quote: Originally posted by tsathoggua1 | 2kg phosphorus (red)
100g cinnamyl chloride
100ml n-butyric anhydride
20g Li metal, or may have been 25g
500g iodine
5g 3-fluoro-4-(1,1-difluoromethoxy)-5-methoxybenzaldehyde
250g n-dodecanethiol
500ml SOCl2
1l nitroethane
Couple of welding-size argon cylinders and 1 of CO2
2l 98% H2SO4
(unsure of the weight, came from a pet store) bottle of methylene blue solution)
500ml conc. HCOOH
And not bought, but a script from my dr. for KMnO4. Needed a portion of one tablet for my foot, to bathe it in, but given a few pots. I am not going
to turn that down. In fact I'm going to shoot for getting it on repeat
Not too familiar with base piranha, never used it. But with the acid version make sure there are no organics left. It'll oxidize inorganic carbon to
CO2 and there is the potential (probability?) for anything but the tiniest traces of organics to result in a nasty explosion. Not a pretty thing to be
covered by conc. H2SO4 and H2O2
[Edited on 9-2-2017 by tsathoggua1] |
Where do you drug chemists get such quantities of phosphorus and nitroethane?
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I wonder if tsathoggua1 is coming back. My guess is that the authorities got a tip from the pet shop owner after his methylene blue purchase.
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CalAm
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5L 50% Hydrogen peroxide
5L 98% H2S04
5L 70% HNO3
500g Phosphorus, red
50g Phosphorus, red sealed under argon in an ampule (desk display)
500ml 65% Oleum
and a fritted buchner funnel 350ml 24/40 + 1L Erlenmeyer flask with a hand vacuum pump from deschem
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tsathoggua1
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Tsath' isn't coming back. He didn't go anywhere to begin with. Did have some confusion with forgetting the password to another account, 'toady' but
just made this account, and before anyone discounts me as some trailer park redneck meth cook, I'm far from it. Won't say I have any problems with it,
not on ethical grounds at least.
But as to whether I'm coming back. No. I'm still here.
And the pet store owner...why would methylene blue..yes its active as an MAOI (MAO-a selective) inhibitor, but generally speaking, of those reagents,
methylene blue is the very least suspicious of the entire lot, more or less. And besides, he makes enough off me when I come in, IIRC my last purchase
of chemicals, tubing, air diffusion stones etc. and assorted things like a long, flexible double-ended (two sizes) brush on the end of a coiled up
wire braid type thing, perfect for scrubbing things out of flasks, cleaning test tubes and what have you. All in all came to £70-something. So he's
got a fair incentive not to go snitching at the purchase of a bottle of dye, for microscope sample staining etc.
The compressor is the blue boxy looking thing,
Guy in this particular pet shop is quite happy to help out. Last time I saw him, he even donated me a fairly powerful air compressor and didn't mind
me going round all the tubing to see which size fitted my Dimroth condenser and one of the Liebigs.
He'd happened to get this pump, someone sold it him in exchange for store credit, but as it happens, its former use was some medical purpose, came
from a hospital, perhaps for CPAP, and it gives off quite a lot of vibration, which made it unsuitable for aquaculture. So he sold it me for the price
he gave away in exchange for someone getting a couple of tropical fish. Kind of an xmas gift, sold at total cost of a fiver.
Oh and this isn't actually my lab itself. Its where excess items have had to find other places to be put, for capacity reasons since I have more
equipment and reagents than I have shelving and bench space. Some of it has to go elsewhere when not in use.
[Edited on 18-2-2017 by tsathoggua1]
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JJay
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Glad you're still with us I wouldn't dare order 2 kilograms of red phosphorus.
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tsathoggua1
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Well 1kg was the minimum order. And buying 2kg meant a modest discount on the total (90 euro/kg). Wanted a fair bit for three reasons-partially an
investment, partly for chasing down as many of the stable, storable allotropes as possible and partly because its just such a damn useful reagent, as
either red or white P, since its fairly easy to produce WP from RP, via distillation under a current of inert gas and collecting the product under ice
cold H2O, melting smaller pieces of WP together if necessary. It can, if ice-cold, below its autoignition temperature, be quickly taken out of the
collection vessel and melt-cast under water for storage, or stored in lumps under degassed, argon-sparged H2O, with the headspace in the container, if
any, likewise given an argon purge.
First intended use for it is to synthesize violet phosphorus, then PBr3 or PCl3 and attempt to precipitate out Schlenk's phosphorus, the allotrope or
polymorph known as scarlet phosphorus.
Not sure if violet P requires white or red, but the basic idea is to recrystallize it from molten lead, after keeping a quantity of elemental P in the
molten lead for around 24 hours, then dissolve away the lead using nitric acid, leaving behind violet phosphorus, otherwise known as Hittorf's
phosphorus. Its fairly unreactive as far as I'm aware .Nontoxic, crystalline, and of all the allotropes, closest to black phosphorus in nature,
although with a polymeric, puckered chain-like structure somewhat similar to red P, although the chain structure is different.
I've read of its synthesis this way using red P. But given red P is a powder, if possible, I'd sooner use WP, since it can be melt-cast, so as to try
and obtain the violet P in large single crystals. Its not commonly available, but the few times I've seen samples of violet P on ebay, its gone for
something like £20 a gram. And that was in the form of a few crystalline chunks.
Since red P changes to the white allotrope under heating, I should think that in a bath of molten lead it would change to WP anyway, would it not? so
why not attempt the growth of large, single crystals using pre-cast pieces of white phosphorus? given how much a few measly looking chunks, equating
to 1g were selling for on ebay, the one time I've seen it available, I'd think large, carefully grown single crystals would go for quite a bit for
collectors seeking element samples.
As far as watched chemicals go, there are a few I wouldn't order, such as 1-phenyl-beta-nitropropene (I've seen it go in 'kits' on ebay including
HgCl2 enough for an amalgam reduction...sheesh), P2P, MDP2P, but generally speaking, I'll order what I need for whatever I'm doing. Really REALLY hot
chemicals like the substituted benzaldehydes, I'd only order from certain sources who won't blab. If needs be though I can order those along with
nitromethane/ethane, and one particular source only, perhaps two, that I'd order that kind of thing together, if I wanted them mind you. I don't go
by other's opinions of what chemicals should and shouldn't be in a hobbyist's lab, bar a very few, which I'd have to synthesize myself.
[Edited on 18-2-2017 by tsathoggua1]
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tsathoggua1
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To be honest, the red phos/I2 reduction of ephedrine/pseudo (its a LOT easier to obtain in england, simply pharmacy only and behind the counter), the
RP/I2 reduction is harsh and ugly. Best way to do it IMO is an in-situ birch-benkeser reduction, using anhydrous gaseous ammonia as a constant stream
into a cryo bathed flask (salt, CaCl2, MeOH, a little H2O and diethylene glycol will get to the point where ammonia is JUST short of liquefaction.
Suspension of Li in anhydrous diethyl ether or diisopropyl ether, I've heard of it being done in hexane also, good stirring then once the blue has
formed (a DROP or two of iPA helps it seems), it first goes dark greenish blue, then forms a proper solvated electron solution in the ether, needs a
constant stream of ammonia, until the blue solvated electron solution is preformed. Its far more tolerant to gaaks in the pseudo.
And why can't amphetamines be synthesized in a home lab (from a chemistry point of view) those P2NP/HgCl2 'kits' are little different in principle
from the old GHB kits when GHB got banned but GBL was legal. IIRC DIY kits with the stoichiometric quantity of NaOH and GBL were sold. This is no
different, the HgCl2 is intended to be reacted with Al to form an Al/Hg amalgam which will reduce the nitropropene straight to amphetamine. Or
reductive amination using in-situ nitromethane would give methamphetamine, or if nitroethane is available then N-ethylamphetamine.
And there are plenty methods to do it that do not require Hg. Such as Fe/HCl or Zn/HCl reductions. Or for the better equipped, catalytic hydrogenation
with platinum group metal catalysts, raney nickel, etc. Or best of all, cleanest and reliable, LAH/THF.
And actually making the nitropropenes, nitrostyrenes is very easy. TETA (triethylenetetramine) works excellently at least on nitrostyrenes with an
electron-donating group on the 4-position, never tried it on any benzaldehydes with extremely electron-withdrawing groups. But TETA in GAA/iPA and the
nitroalkane of choice to form either the nitrostyrene or nitropropene, these are insoluble in H2O, so pouring onto cracked ice, straight from the
finished rxn will crash the nitroalkene out, then ice cold H2O washing for workup after filtration, followed by recrystallization from iPA or MeOH to
remove the pumpkin orange byproduct gives good quality nitrostyrenes.
IIRC, although never done it, another excellent way is to reduce with first a dissolving metal reduction to the amine then reduction of the double
bond with borohydride.
And thats starting from benzaldehydes. If one wanted simple benzaldehyde, the Etard reaction using chromyl chloride can be done on benzyl alcohol or
toluene.
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tsathoggua1
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Quite. Certainly those packages with the HgCl2 and 1P2NP, there is no way in hell I'd order that from ebay. There is only one supplier I have I'd
trust with that kind of order. Better to buy the substituted benzaldehydes and do a Knoevanagel. Getting to the nitropropenes and nitrostyrenes is
easy as it gets. Probably one of the easiest organic reactions, bar maybe synthesis of bromethiazole/chlormethiazole I've ever done.
Those nitropropene packs look too much like bait to me. And I'm not biting. Benzaldehyde itself is cheap enough and FAR less on top. Benzaldehyde,
EtNO2 in GAA with TETA, done in a few hours. The reductions are the more challenging part, some of the dissolving metal type (acid/metal rather than
Birch type) reductions IIRC don't work on nitropropenes, only on nitrostyrenes. Damned if I can remember which ones though. LAH is the way to go
though, although for the 3-bromo-4-(1,1-difluoromethoxy)-5-methoxybenzaldehyde project, Red-Al is going to be used, even on the nitrostyrene.
Off topic sort of-but are the nitropropene reduced products racemic when using LAH?
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tsathoggua1
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Does anybody have any suggestions for UK located suppliers of semi-bulk quantities of solvents (10, 20 liters) for things like diethyl ether, MeOH,
acetone, MEK, iPA, toluene, benzene, diisopropyl ether (I'm sick and tired of having to fractionate DIPE based starting fluid, to remove toluene,
heptane and acetone), could use a good source of acetonitrile, EtOAc, DMF and HMPA, as well as carbon disulfide and carbon tet, chloroform, CH2Cl2 and
other chlorinated hydrocarbon solvents. Also, aliphatics, pentane especially, its one of my favoured solvents for quite a lot of things, especially
recrystallizations since it can be stripped so rapidly.
I'm having especially a lot of trouble finding HMPA, CS2 and chlorinated hydrocarbons are a fucking nightmare now to source. AFAIK in the UK all OTC
products formerly based on dichlor are things of the past now, thanks to big brother and the nanny state.
Oh and I still don't get why buying methylene blue would be suspicious. Sure, its bioactive, as an MAOI, but thats hardly a reason for someone to call
the filth if they were that way inclined. I doubt the pet store owner even KNOWS what an MAOI IS for that matter.
[Edited on 19-2-2017 by tsathoggua1]
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tsathoggua1
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I wasn't claiming to be one. I was merely remarking about the greater feasability, from a tech point of view of starting from the benzaldehyde. The
reaction, such as if one wants to stay legal, producing unsubstituted phenethylamine, is not difficult.
And I was more commenting on how blatantly bait-ish those direct precursors are, especially when sold with the HgCl2. Thats about as blatantly obvious
as one can get, as there can't be that many other uses for a pack of 1P2NP and HgCl2. The HgCl2, sure, but not the nitropropene. Damn.
And the solvents, well, I just need to restock, because I am running low on everything. Have had to resort, for EtOH to distilling cooling spray,
separating off pentane and a little menthol.
The particular benzaldehyde mentioned, well, thats not something done for profit, its a very small scale research project, because I have been unable
to track down any such derivatives with an electronegative substituent on the 3' carbon of the phenyl ring. And you can bet with the availability of
the aldehyde of 5g total at a cost of £80-something, I am not setting up the next pickard-esque factory. I'm genuinely interested in the pharmacology
here, not just making bulk amphetamines. I could do that with sources I have, IF I were so inclined. Too easy, unless theres some exotic chemistry
involved, new routes etc.
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JJay
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I ordered some tartaric acid for making Fehling's solution
My, we are having lovely weather today
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tsathoggua1
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I need to buy a new alembic. Just had mine crack. And unfortunately, it was full of white phosphorus. Was doing a distillation, and due to the
breakage, it started bursting out in little sparks of glowing intense fire, until I put an argon tank to the crack, took it over to water, and since
it was fucked anyway, cracked it open. Didn't manage to recover more than a tiny bit though. On the plus side, the side-arm survived in one piece, so
I can at least fuse it closed and do it in a sealed tube to prepare some more.
No rest for the wicked. Lost a fair bit of red P as well, in the form of solidified lumps of partially red, partially white (it was pyrophoric, but
looked mostly red, like solidified lumps of clay) Managed to salvage a small amount. About half a pea-sized from a generous heap (unweighed) to about
1/5th fill the alembic, started roasting it and the damn thing bulged outwards. I'm thinking it might not have been borosilicate glass.
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CalAm
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Speaking of odd chemicals found on ebay tsathoggua1, i stumbled upon a seller stocking quiet the array of precursor or otherwise hard to find
chemicals. I would have to hope it is a honeypot ? I mean who else would advertise: LiAlH4, HF(70%), Oleum, Phosphoric acid 85%, Ammonium Chloride,
phosphorus, Hydrogen Chloride gas, Palladium (II) Chloride and a whole range of other wonderfully hard to get items all posted to you from Kekava,
Kekava region, Latvia.
I am unsure if i am able to post a link to their ebay store ? So if someone could inform me if it is okay to post it here i am sure you guys will have
a chuckle as well.
[Edited on 19-2-2017 by CalAm]
[Edited on 19-2-2017 by CalAm]
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elementcollector1
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Sounds like yet another sting operation to me. How would one even sell hydrogen chloride in gaseous form? In a steel tank? That's not exactly cheap or
helpful.
EDIT: I'm not sure you should post that link either, to be honest. Not knowing what's going on with that site, I can't say for certain.
[Edited on 2/19/2017 by elementcollector1]
Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
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JJay
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I bought some distilled water. I paid cash and didn't answer any questions. The cashier was being all nosy, asking things like, "Hi, how are you?" but
I don't think she suspected that I was doing any chemistry, and I switched trains twice on the way home.
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