Polystyrene foam and acetone ==> P2P

java · Consumer

Shane_Warne
(Newbee)
05-31-04 20:33
No 510625




Polystyrene foam and acetone ==> P2P
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It's a more worthy project than a biosynth, isn't it? More predictable.outcome.

I know a lot of bees here think that they're only capable of doing RP/I2 reactions, thus ephedrine is the only goal.

Polystyrene foam --(heat)--> styrene monomer--(95C, ammonia water, sulfur, EtOH)-->Phenylacetamide--(hydrolyze using base or acid)--> phenylacetic acid

Acetic anhydride comes from ketene produced by from tone and a ketene lamp. (UTFS for ketene)

phenylacetic acid + acetic anhydride ==> P2P

P2P + Al/Hg salt and methylamine ==> ----

Post 495436 (tweekdexter: "new preparation of phenylacetic acid", Chemistry Discourse)
Post 258134 (foxy2: "New preparation of phenylacetic acid", Chemistry Discourse)

What do you bees say?

cycosyince
(Stranger)
05-31-04 23:17
No 510657




thats it?
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So there is a smattering of interest, yet the other curiosities beg to bee addressed, such as: Little detail as to have you actually run this synth?
What kind of problems are inherent with it?
What kind of ratios/yeilds are we gonna find?
What kind of time is involved?
how much equipment will it require?
Can it be done ala ghetto without an added risk to factor?

Impress the bees with the rundown, not just a tease...
VE could learn you a thing or two about throwin down new techniques on the forums.

YOU have the floor,
we're waiting...

uh, you know, stuff.

Shane_Warne
(Newbee)
06-01-04 04:10
No 510683




I don't care...
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If you sink, and surely burn.

If you had read the experimental you would have discovered a 60% yield of phenylacetic acid from polystylene is really, realistic.

The downsides are smell at various stages. WizardX said that the smell of sulfur, during the step from styrene monomer to phenylacetamide would bee quite disturbing.

But it's unclear to me whether WizardX considered sealing the vessel as the guy in the experimental did.

The time factor is dependent on your knowledge and workmanship. It could take monthes, or it could take years.

What kind of ratios/yeilds are we gonna find? Read/UTFSE

Can it be done ala ghetto without an added risk to factor?

Hard to say. purifying the styrene monomer requires fractional distillation, but because it's acidic, I doubt a copper setup would suffice. We have to investigate this. So ar you gonna help or just bee a dick?
The methods are very well established, we just have to work out how to make them suitable for us.

Turning the styrene monomer in to phenylacetamide, and then on to phenylacetic acid, one of the two main ingredients to P2P requires no lab equipment, as you would discover if you had clicked the link I searched for YOU.

Al/Hg requires Aluminum sheet, either foil or Al from cans that have been well cleaned (sanded).
Hg from mercury that has been treated with chlorine gas. small amounts of the Hg salt are reuired for reductive aminations.

Buying pills is a trap. Whether one does it him/herself or has a whole hoard of people buying them.

The smart money is on P2P.

Oh and it's not a write-up, it's a life-line. But VE is welcome to add to our project.

Come on, don't be a fag nowe, we require a ghetto method for phenylacetic acid, and acetic anhydride. Both have been described here at The-Hive first hand.

Ill keep reading.

ApprenticeCook
(Hive Bee)
06-01-04 08:35
No 510712




Re: Buying pills is a trap.Getting that ...
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Buying pills is a trap.

Getting that way.... so yes i do agree buying eph is going out... p2p needs to be the way to go...

This sounds too good to be true... but reading the info it sounds rather good and not too hard...

Its just my opinion, but no-one listens to me anyway, and rightly so...

Organikum
(Wonderful Personality)
06-01-04 10:46
No 510730




No need for polystyrene pyrolysis
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Styrene monomer is in polyester resin - usually 40% to 60% depending on the manufacturer, no need to pyrolyse polystyrene.

On my desk before me sits a box of usual car-repair polyester resign, 242gram. It says: 46% styrene content, which should be easily recovered by plain distillation, whereby it is questionable if this is even necessary for the following sulfur treatment - the mix contains probably some polymerization inhinbitors which might come handy.
With the box come about 8 gram dibenzoylperoxide a polymerisation catalyst which is useful as a radical initiatior in many other synths (chlorinations based on radical substitution mechanism for example, like toluene to benzyl/benzalchloride and more).
It wont be 8 gram peroxide plain, but X gram + solvent of course but this wont matter much for the intended uses.
Both, resin and radical initiator can be bought as single compounds. Even styrene pure as solvent for plastics is available for everybody who looks around a little bit. It is not forbidden to build oneself a surfboard by now.

hope this helps
ORG

PS: Before doing the pyrolysis of acetone I would suggest to have a look into the reactions of acetic acid and phenylacetic acid to yield P2P. This seems to me favorable over acetic anhydride pathways.

Schnabufugl!

xxxxx
(Hive Bee)
06-01-04 11:18
No 510732




maybe even less difficult?
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i once saw a quart of pure styrene monomer for us$10. for the wilgerodt a high boiling amine can repace ammonia. once you have phenylacetic acid consider maybe ethyl phenylacetate condensed by sodium ethoxide with ethyl acetate in ethanol then saponification and decarboxilation to form p2p?

WizardX
(Wizard Master)
06-01-04 22:04
No 510824




Work Up?
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The downsides are smell at various stages. WizardX said that the smell of sulfur, during the step from styrene monomer to phenylacetamide would bee quite disturbing.

But it's unclear to me whether WizardX considered sealing the vessel as the guy in the experimental did.

At some point you must open the reaction vessel to work up the reaction mixture. This is where the pungent sulphur smell is.

ApprenticeCook
(Hive Bee)
06-01-04 22:15
No 510828




sulphur is rotten, so thats a problem but what
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sulphur is rotten, so thats a problem but what about yields etc??? is this process worth the smells it produces by creating some nice clean p2p (after disto) in decent yields?

Its just my opinion, but no-one listens to me anyway, and rightly so...

WizardX
(Wizard Master)
06-01-04 22:42
No 510836




PHENYLACETAMIDE
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PHENYLACETAMIDE: http://www.orgsyn.org/orgsyn/prep.asp?prep=cv4p0760

Phenylacetamide has been obtained by a wide variety of reactions: from benzyl cyanide with water at 250ñ260?;5 from benzyl cyanide with water and cadmium oxide at 240?;6 from benzyl cyanide with sulfuric acid;7,8 by saturation of an acetone solution of benzyl cyanide with potassium hydrosulfide;9 from benzyl cyanide with sodium peroxide;10 by electrolytic reduction of benzyl cyanide in sodium hydroxide;11 from ethyl phenylacetate with alcoholic12 or aqueous13 ammonia; from phenylacetic acid with ammonium acetate14 or urea;15 from diazoacetophenone with ammoniacal silver solution;16 from phenylacetic acid imino ether hydrochloride and water;17 from acetophenone with ammonium polysulfide;18 from benzoic acid;19 by heating the ammonium salt of phenylacetic acid;20 and by heating cinnamic acid with a mixture of sulfur and ammonium hydroxide.21

Shane_Warne
(Newbee)
06-02-04 05:31
No 510901




Life's alright!
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Organikum, your right, styrene momoner is out there in resins and readily available, as is every other ingredient.

Post 489377 (Organikum: "Another way to GAA", Chemicals & Equipment) Acetic acid from vinegar... A better method
GAA (Glacial acetic acid) from acetone vapour decomposition to ketene, using a Cu tube and a burner, then bubbling the produced ketene through a 70C solution of vinegar, to form acetic anhydride, hence reacting with water to form GAA, simultaniously distilling off acetone that isn't successfully decomposed by the pass.

ORG is there any problems with this setup, that swiO has discovered?

Flash back problems when the acetone exits the aspirator tube and the GAA reaches a flammable concentration? (despite the vacuum)

The connection from the end of the bubbling tube to the vinegar flask (?) sounds like it would need more than a rubber stopper, any ideas?

ORG your right, a route from acetic acid would be preferable and more straight forward. I mean, the route from acetic anhydride isn't bad by any stretch of the imagination, and is worthwhile and realistic, but concentrating a solution of acetic acid is just more straight forward.

Also if you have phenylacetic and GAA you can use any procedure which use phenylacetates and acetates too, which don't require high temperatures, if one has that limitation...

Post 23796 (Mastermind: "Re: P2P", Methods Discourse)
'...A mixture of PAA and acetic acid was passed through the tube at around 400-450C ... P2P'

WizardX, thanks for dropping by to say that. I just wasn't sure if you had considered a sealed vessel or not.

WizardX and ApprenticeCook, perhaps we could consider cooling the vessel down to room temperature, and then freezing the vessel before work-up to lower the sulfur stench.

There's always a fumehood too.

Ill dig up the yield numbers, what numbers do we need need...

from acetone -> acetic acid or to acetic anhydride
from styrene monomer --> phenylacetic acid
from phenylacetic + acetic acid OR acetic anhydride --> P2P
from P2P -(Al/Hg)-> ----

What about the yields of P2P using acetates and phenylacetates that you can make with your acids, are you guys interested in those too?

We can way them up then.

I'm pretty sure I2 or KI from RPI can be used to form a Hg salt too btw, instead of Cl, so there's no worry about Cl gas, and it's just neater.

Organikum
(Wonderful Personality)
06-02-04 07:41
No 510935




Yes, I was referring to masterminds tube with...
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Yes, I was referring to masterminds tube with MnO catalyst, this plain eliminates one step (acetone to AA) and is IMHO favorable.

The use of the mercury iodide was covered already but not everybody got it going as far as I remember.

Schnabufugl!

ning
(acetaminophanatic)
06-02-04 22:55
No 511145




Stink
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I wonder what would happen if one were to add H2O2 to the reaction vessel and stir well before opening it.

H2O2 will oxidize sulfide ion to elemental sulfur. It is used industrially to do this in the treatment of wastewater and sewage. It shouldn't have much effect on the phenylacetic acid.

This will also make the workup hydrolysis not emit poisonous H2S fumes, hopefully. An important factor for the larger-scale cook.

We'll all meet someday...on the other side

Chewbacca
(Hive Bee)
06-03-04 06:29
No 511200




innovative
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such an idea would also be useful for any other reaction in which a side product is H2S.. bubble into H2O2.

The shit we go through to get high...

Organikum
(Wonderful Personality)
06-03-04 07:37
No 511209




smells
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Also if you scavenge the sulfur stink from hell - there will be always left the sweet smell of phenylacetic acid. "Sweet" is of course relative. VERY relative.

Schnabufugl!

Shane_Warne
(Newbee)
06-03-04 13:53
No 511266




yields and talk
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Ning: The H2O2 sounds good!

The yields are extremely high to phenylacetic acid, well in the patent that ning translated in the other post it is reported as such. Ill paste it here to help with organisation.

In a reaction vessel was placed:

Styrene 21.7 g
Sulfur 37.6 g
Ammonia 50 ml
Ethanol 30 ml

'Under stirring and heated at 93-95 C for 3-4 hours. Fluids were evaporated from the mixture, it was allowed to cool, and extracted 3 times with 500 ml hot water. The decolorized solution after standing yielded 26.7 g (97%) white sheets having MP of 157-158 C and BP of 280-290. (Phenylacetamide C8H9NO)

100 g of the above phenylacetonitrile and 80 ml HCl were added to 150 ml water and refluxed for 2-3 hours. After cooling to room temp, a precipitate formed and was filtered and recrystallized from 1:2 ethanol/water to yield 84 g (84%) of shining white crystals. (Phenylacetic acid C8H8O2)'

So it works out to about 90% from styrene monomer to phenylacetic acid. That's fucken good for 2 steps and OTC ingredients.
Knock a big fat 30% off that, and we're really in the realistic (pesimistic) zone, and it's still very nice.

Ac2O (acetic anhydride) or AcOH (acetic acid) seem to be the hardest, and the most fiddle to setup an apparatus.

Dangerous too, ketene is deadly and flammable, but won't explode if O2 is absent (same with acetone)

Also although acetone is cheap, it isn't expendable IMO, and it wouldn't surprize me if it disappeared at some point. I hop not, but you have to plan for the worst.
So having an implementation in your aparatus to save acetone that isn't successfully decomposed is almost essential.
Dripping acetone on a glowing toaster wire inside a copper tube should do the trick. Bubble the ketene produced through a hot flask or jar of vinegar, fitted with a two-hole teflon-coated cork.
The 2nd hole leads to a jar sitting in ice to condense the acetone that distills off the first jar.
Still I've never done it, but that's where my thoughts start.

Oh, boys! I've got a phat surprICE for ya! If you can't acquire methylamine, or just don't want it around, you can have plain amphetamine from the Al/Hg, in high yields (96-98%), using only 25% ammonia water.
See for glee: https://www.rhodium.ws/chemistry/amph.alhg.html
Actually the yield at the introduction of this page is totally different to the experimental, at 30%. I'd trust the 30% as more realistic

The yields of P2P from PAA and AA, with NaOAc aren't very good, and a large excess of AA is used (to avoid useless dibenzyl ketone formation, it states) , but even then, 50% is optimistic.
Read for yourself here: https://www.rhodium.ws/chemistry/phenylacetone.html--phenylacetic
A longer reaction seems important for yields too.

ORG:
There isn't much info on methods that use acetic acid instead of acetic anhydride. Sure there's that Mastermind post, but what is that worth? What guidance is it? Ill try find more but I think it'll turn out to be more wise to put the effort in to acetic anhydride, don't you think?

randolph_carter
(Hive Bee)
06-03-04 14:16
No 511267




sweet smell indeed!!!!
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that is one way you "could" describe that smell!!!

if one is into dreaming about this particular molecule (paa) they should be prepared for the almost unremovable "sweet" smell that this compound imparts to almost everything it touches.....

wearing tyvek coveralls is DEFINITELY recomended so ya can burn em.....

all work surfaces should be covered with plastik for disposal....so ya can burn it.....

gloves will stink to high heaven forever so use , you got it, disposable gloves......so ya can burn em.....

this is one of the more tenacious smells that some swinoidz back in the day of paa-acetic anhyd-pyridine synths of p2p became quite adept at picking out...

i once overheard one of them referring to someone who had came in to the local zippy mart with that smell on them as "having the sweet smell of success..." and i read about the poor soul in the newspaper the very next week and it wasn't because of particapatin in a 4-h project why he was in the local paper...

just a lil heads up for people who are unaware of this issue....

YOU WILL GET IT ON YOU!!!!!
YOU WILL FIND IT VERY DIFFICULT TO REMOVE FROM YOU!!!!!!
SWINOIDZ DO KNOW WHAT THAT FUNNY SMELL IS AND WHAT YOU MAY BEE DOING WITH IT!!!!!

just take appropriate precautions to avoid this problem....
fyi...

"remember little ones, love is real,not fade away, so pass some ammo on today......"

Organikum
(Wonderful Personality)
06-03-04 17:49
No 511299




Re: you can have plain amphetamine from the...
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you can have plain amphetamine from the Al/Hg, in high yields (96-98%), using only 25% ammonia water

Thats sadly not true.
If you know a trick which makes this possible please tell! It would be highly appreciated.

For the rest: VERY GOOD! A real breakthrough!

ORG

Schnabufugl!

DrLucifer
(Hive Bee)
06-03-04 22:13
No 511335




Antipolymerization agents...
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In regards to distillation of polystyrene, swim feels that a vital element is missing from discussion!
That is of course, the antipolymerization agent required for the final stage of the Polystyrene-->Syrene reaction.

Preparation of styrene:
A distillation setup was assembled and 100g of powdered scrap polystyrene was added and heated to 340 C or higher. The distillate over 340 C was collected and assumed to be styrene. Still, the color was rather crimson, and impure. The impure product was mixed uniformly with 5% by volume sulfuric acid and was left to stand for 3h to remove impurities, then rinsed 3 times with brine, dried with anhydrous sodium sulfate, added antipolymerization additives.
The portion boiling at 145-146 C was collected to yield 89 g (89%) styrene.

This text is fresh from translation, but you get the idea.
Now, whilst swims initial searches didnt fruit anything terribly useful, he did find out that methanol is incorporated into embalming fluids as an antipolymerization agent for formaldehyde.
Im not sure whether methanol would be suitable in relation to crude styrene, but swim figures it is worth trying.
Can anybody suggest a better antipolymerization agent?
Would different agents affect the boling point of the styrene?
Another question would be what concentration of H2SO4 is required in this process? Swim would assume that 5%/volume of 98% H2SO4 be used, but since its role is to remove impurities, perhaps more/less could be used depending on how well the initial distillation proceeded...
Now despite the styrene monomer being available commercially, swim feels the route from polystyrene would be more practical to start with!
What are bees opinions on this subject?

I'm a diamond that is tired, of all the faces i've aquired.

Shane_Warne
(Newbee)
06-04-04 00:08
No 511346




oh no, a mistake?
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ORG, I'm looking at that experimental page again and I can't see the error in the reagents or the product.

phenylacetone (P2P) + Al/Hg + EtOH + ammonium hydroxide --> Amp!

The yields in the introduction don't seem to correspond at all to the experimental section, neither does the explanation on that page, about yields.

Is it the yields that aren't true, or the procedure just doesn't work, or have I missed something?

talking about it is the breakthrough.

randolph, could you quantify the smell even further by comparing it, to say aromatic hydrocarbons and iodine?

Anyway, the task is worthy of an exaust fan and a carbon filter, but just for interest.

I can see what your saying too, there will be a smell because it states that the '...Fluids were evaporated from the mixture, it was allowed to cool, and ...'

DrLucifer, I don't know but I hope someone does. no point in bullshitting on purpose.

weaz1dls
(Hive Bee)
06-04-04 04:29
No 511397




Go Shane GO
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Impresive, mostly over SWIW's head at this point. Did wonder if anyone was going to address the smell factor. Will contact an old Bee who's old lady had some spray shit she would make. Sprayed onto surfaces in hotels it nutralized that shit. SWIW is sure someone here could figure it out. Ok enough cave chater Swiw will read up here and attempt to get on the same page. Any 101 links PM'd in relation to the mechanics would be helpful.

josef_k
(Hive Bee)
06-04-04 07:30
No 511433




Re: The yields in the introduction don't seem...
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The yields in the introduction don't seem to correspond at all to the experimental section, neither does the explanation on that page, about yields.

Is it the yields that aren't true, or the procedure just doesn't work, or have I missed something?

If you look more closely you can se that they got 12.5g (0.09 mol) amphetamine from 40g (0.3 mol) phenylacetone. About 30% yield. That bit about 98% yield is probably the yield of amphetamine sulphate from amphetamine freebase.

Rhodium
(Chief Bee)
06-04-04 13:01
No 511472




Reduction: 30% Crystallization: 96-98%
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josef_k: You've interpreted the article correctly - maybe I should clarify that in the document so that people don't mislead themselves.

The Hive - Clandestine Chemists Without Borders

Shane_Warne
(Newbee)
06-04-04 22:48
No 511565




thought so
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I thought it could only have been the yield.

The amount of acetic anhydride or acetic acid to phenylacetic acid, for a 40-60% yield by experts with all the best equipment makes it less attractive.

But the apparent ease of preparing phenylacetic acid from OTC ingredients in high yields make that a good starting point. agree or disagree?

So we need a high yielding method that uses phenylacetic acid and a cheaper, more easily prepared 2nd reagent to yield P2P. yes or nah?

There's this one. That yields about 70%, but the methyllithium, requires methanol to prepare methyl iodide to prepare the methyllithium I think.
If you can acquire methanol, a bit of red phosphorus and KI, then this is for you. SWim personally has never had use for methyl alcohol, just methylated spirits and iso.

https://www.rhodium.ws/chemistry/p2p.paa-meli.html

This following one uses calcium phenylacetate and calcium acetate, and the amount of acetic required (as calcium acetate) is much less.

https://www.rhodium.ws/chemistry/p2p.paa-ca.html

Any thoughts on some others bees?
Because the route to P2P from phenylacetic is what's going to get you high the following week. It's best to think about it sooner rather than later, or else it's:

Pills and pain.

foxy2
(Fragile ego)
06-06-04 05:36
No 511756




added antipolymerization additives.
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added antipolymerization additives.

TBC (4-tert-ButylCatechol), BHT (butylated hydroxytoluene), TBHQ (tert-Butylhydroquinone) or (BHA) butylated hydroxyanisole are examples of some common polymerization inhibitors that should work. Hydroquinone and other free radical scavengers might work also.

http://www.democracynow.org/ - The Exception to the Rulers

ning
(acetaminophanatic)
06-06-04 12:35
No 511806




Exactly
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And given its tendency to be oxidized, I wouldn't bee surprised one bit if acetaminophen might substitute for hydroquinone in a pinch....

I read somewhere that calcium acetate can be used to produce p2p from phenylacetic acid. This is a much more attractive option to my mind than lead or acetic anhydride.

Perhaps one could perform the operation sequentially--after acidic hydrolysis of phenylacetic acid and H2O2 precipitation of sulfur, the mixture would be filtered to remove sulfur, leaving a mixture of ethanol, water, ammonia, hydrogen peroxide, and phenylacetic acid.

A small amount of copper sulfate or MnO2 (or KMnO4) would be added, to catalyze the destruction of the remaining H2O2, (either turning it to O2, or oxidizing the ethanol to acetic acid), then the requisite amount of calcium base (lime or chalk) could be added, and an appropriate quantity of vinegar, and the whole shebang distilled to remove all fluids. This would strip off the ammonia, alcohol, and water. Then, once the last bit of water left, the reciever could be changed, and a vacuum applied. P2P would start to be collected, until the reaction completed.

Since this implies even a one-pot reaction is possible, it might minimize contact with the foul phenylacetic acid. No acetic anhydride necessary.

One might be tempted to take the p2p collected and throw in some oxalic acid or formic acid and ammonia, for a leuckart reaction, following Zealot's fine instructions. How delicious!

Well, that's enough wild speculation from me

We'll all meet someday...on the other side

pink_dust_angel
(Stranger)
06-13-04 13:40
No 513182




what exactly does the sulphur do in this ...
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what exactly does the sulphur do in this reaction..ive seen the Willgerodt reaction but this reaction is not a Willgerodt as i understand.if the sulphur is turned to H2S then im ok..can some knowledgable kind person give a balanced equation?
yes i did check all the posts but only one i found that had equations(apprently) was a dead link

ning
(acetaminophanatic)
06-13-04 19:30
No 513223




It is.
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Go look on rhodium's page. You will see that they are the same.

If one were to use another oxidizer along with the sulfur (like H2O2), then it would be a "catalytic transfer wilgerodt reaction", operating in much the same way as a wacker oxidation, with the sulfur temporarily being reduced to H2S before becoming oxidized back to sulfur again.

Since the wilgerodt reaction works on all manner of materials, including alkenes and alkyl ketones, I very much suspect that it would work with H2O2 included. Would be fun to try.

Also, I don't think the reaction emits H2S vapors during the oxidation even though it is generated during the oxidation of styrene, because the H2S reacts with the included ammonia to form ammonium sulfide. When the reaction mixture is hydrolyzed and acidified is when the H2S should be released, so addition of oxidizing agents to the hydrolysis to scavenge the H2S as it is released should take care of the major smell component (I hope)

The wilgerodt is potentially very OTC and bulk-capable, so I think it deserves some careful attention.

Clandestine chemist // amateur pharmacologist

callen
06-13-04 19:36




P2P...the old way
(Rated as: misinforming)
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pink_dust_angel
(Stranger)
06-14-04 04:37
No 513287




ok ive checked 3 organic text books and 1...
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ok ive checked 3 organic text books and 1 inorganic and there is nothing in any of them about Wilgerodt-Kindler
wilgerodt or kindler....i googled Wilgerodt-Kindlerand got 3 results non of which gave a reaction mechanism or anything of the sort.
the thing thats confusin me is that the Wilgerodt on rhodium shows the compound produced to contain sulphur while the one on this thread seems to produce simple phenylacetamide......

Osmium
(Stoni's sexual toy)
06-14-04 05:19
No 513293




That's why spelling is important.
(Rated as: good read)
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That's why spelling is important.

http://orgchem.chem.uconn.edu/namereact/willgerodt.html
http://fachschaft.cup.uni-muenchen.de/~schleifi/reaktion/reaction/willgero.html

http://www.google.com/search?q=willgerodt

BUSH/CHENEY 2004! After all, it ain't my country!
www.american-buddha.com/addict.war.1.htm

Organikum
(Wonderful Personality)
06-14-04 05:41
No 513294




spare the time searching bees
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The link:
Post 282823 (callen: "the "Great Bear" method", Newbee Forum))

Forget it, not worth to look at. This was covered better all over.
ORG

Schnabufugl!

Shane_Warne
(Hive Bee)
06-14-04 18:35
No 513408




I read somewhere that calcium acetate can be...
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I read somewhere that calcium acetate can be used to produce p2p from phenylacetic acid. This is a much more attractive option to my mind than lead or acetic anhydride.

Mine too. I wrongly thought that calcium acetate was one of the acetates that was harder to prepare, but it can actually be done with vinegar an CaCO3. Making it the easiest method imho.

But trying to prepare the correct amount, in situ, with unknown % vinegar would be totally rediculous. Especially for beginners. (like swisw)

As far as H2S goes, the H2O2 is a good partial remedy, but because H2S is so dangerous, and such small amounts can be detected, a fume hood with carbon filters should be essential.

Even a nanoscale testrun is going to cause problems with the local inhabitants, I'd imagine. If you've ever accidently left a bit of pfed.sulfate in an RPI then you'll know what I'm talking about.

It isn't difficult finding proper fireproof, and chemical proof fans with appropriate ducting in the one shop.

But about the H2O2, I like the idea myself. So you don't think it would detrimentally effect the hydrolysis at all?

Does polystyrene dissolve in styrene monomer, or are they easily separated if some of it polymerizes?

It'd be cool if your right about acetaminophen/paracetamol ning.

Here's the calcium phenylacetate and calcium acetate reaction again. It requires a really easy fractional distillation of the 3 ketones in produces, one valuable (P2P/benzyl methyl ketone).

https://www.rhodium.ws/chemistry/p2p.paa-ca.html

It needs to be experimented with, to find out what the ratio of the products (3 ketones) typically is. Sounds good anyway.

What does the author mean by, "a sulfur vapor bath"?

ning
(acetaminophanatic)
06-14-04 19:49
No 513416




Hmmm
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Good catch, that link. I couldn't find it

But trying to prepare the correct amount, in situ, with unknown % vinegar would be totally rediculous. Especially for beginners.

I doubt a p2p synthesis is a good idea for beginners anyway. But, umm....at least where I live, all vinegar is labelled with its percentage. 3%, if I remember correctly. It doesn't really matter, because you can always titrate the pH to neutral with litmus paper. Or, to be even easier, if you are using calcium carbonate, just add until there's no more bubbling from CO2. I don't think even beginners would have trouble with that.

But about the H2O2, I like the idea myself. So you don't think it would detrimentally effect the hydrolysis at all?

No. Both phenylacetic acid and p2p are at the highest state of oxidation they can reach by normal means. Only beastly things like boiling nitric acid, concentrated peracids, and permanganate would be able to oxidize them more (and of course molecular oxygen, suitably heated)

Does polystyrene dissolve in styrene monomer, or are they easily separated if some of it polymerizes?

Dunno, but I reckon the wilgerodt reaction will produce enough tar on its own, so I would say just throw the crude styrene directly into the oxidation, then use the fact that the product is an acid and water soluble to effect the purification. I don't think the polymerized styrene's going to affect anything. It's plastic, after all!

I don't even think one would need to call it a fractional distillation...

I hear that the yield in that reaction goes up when it is performed under vacuum to immediately suck up the formed p2p. To something like 70%. Wow.

Really, really, guys. If the twin evils of sulfurous smells and need for pressure in the wilgerodt reaction can bee overcome, I think we have a winner. P2P from plastic. Can it get any sweeter than that?

Clandestine chemist // amateur pharmacologist

Shane_Warne
(Hive Bee)
06-15-04 02:12
No 513493




chatter
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I doubt a p2p synthesis is a good idea for beginners anyway. But, umm....at least where I live, all vinegar is labelled with its percentage. 3%, if I remember correctly. It doesn't really matter, because you can always titrate the pH to neutral with litmus paper. Or, to be even easier, if you are using calcium carbonate, just add until there's no more bubbling from CO2. I don't think even beginners would have trouble with that.

ok ning, you get cute with your one-pot design.

I doubt you'll get it to work though, as you won't be able to see many bubbles as it gets along, especially as the amounts of water increase 10 fold.

As the concentration of your 3% vinegar goes down, CaCO3 and Ca(OH)2 will fail to dissolve, and it'll just sit there.

I've found that usually when making acetates with vinegar, there's usually leftover carbonate, upon crystallization, and it needs to bee recrystallized with vinegar to convert it.

Besides, making it with vinegar (not in situ though) is only suitable for a microscale test run.

Then again, buying vinegar is a lot less unpleasant than buying those aweful pills!@

Dunno, but I reckon the wilgerodt reaction will produce enough tar on its own, so I would say just throw the crude styrene directly into the oxidation, then use the fact that the product is an acid and water soluble to effect the purification. I don't think the polymerized styrene's going to affect anything. It's plastic, after all!

Good! really good.

I hear that the yield in that reaction goes up when it is performed under vacuum to immediately suck up the formed p2p. To something like 70%. Wow.

Do you know by any chance, if vacuum replaces CO2?
Then we'll have: polystyrene foam, vinegar, chalk and a hoover deluxe

Really, really, guys. If the twin evils of sulfurous smells and need for pressure in the wilgerodt reaction can bee overcome, I think we have a winner. P2P from plastic. Can it get any sweeter than that?

Not really, it's a winner. Especially now that we've put pen to paper and sorted out the route to P2P, to move forward on. You've helped a LOT. ORG aswell, and everyone else.

I wonder if a pressure cooker, with it's pressure release valve sealed, would do the trick?
They are normally stainless steel or aluminum alloy.

Osmium
(Stoni's sexual toy)
06-15-04 04:32
No 513519




Why don't you people try out the original...
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Why don't you people try out the original literature synth before getting all excited about the many tweaks and improvements that might (more likely: might not) work?

BUSH/CHENEY 2004! After all, it ain't my country!
www.american-buddha.com/addict.war.1.htm

ning
(acetaminophanatic)
06-15-04 12:18
No 513586




Of course
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That's the natural thing to do. You could help

Since they need the reaction run at 95 C (IIRC), and ethanol boils around 80, it may be possible to achieve the desired temperature using a reflux apparatus. A pressure cooker could very likely do it as well, but of course it would have to be a stainless steel one. (Hot boiling oxidizing mixture, not good) Which might not be such a bad investment, really.

I'd say, try the reflux first. Monitor the bath temperature and see if it can get high enough. If that fails, then go hunting for a pressure cooker.

And I only suggested one pot (actually two pots) might be possible, reusing the same apparatus. Of course nothing is ever quite that simple, but...whatever

Well, rural bees, let's see what ya got!

Clandestine chemist // amateur pharmacologist

pink_dust_angel
(Stranger)
06-17-04 13:21
No 513992




am i correct in assuming that the ethanol is...
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am i correct in assuming that the ethanol is just a solvent in this reaction?am i also correct in assuming ethanol can be reploaced by another solvent like methanol or isopropenol?yah i found the alternate reaction with just (NH4)2S and water (sans ethanol though)

Shane_Warne
(Hive Bee)
06-17-04 16:59
No 514013




am i correct in assuming that the ethanol is...
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am i correct in assuming that the ethanol is just a solvent in this reaction?am i also correct in assuming ethanol can be reploaced by another solvent like methanol or isopropenol?

I'd assume so. The ethanol and NH4OH solution would be good solvents for the sulfur, at elevated temperature and that's probably why they were chosen.

SWIM would just use denatured, because EtOH, straight EtOH isn't common in Oz, and it's just more hassle.

Plus, considering the yields and feedstocks cheap price, other than controlling the smell, there shouldn't bee too many problems.

http://www.azom.com/details.asp?articleID=1177--_Sulphide_Stress_Corrosion

I've never seen a stainless steel that remains stainless for too long.

I suppose you could sit a teflon coated saucepan in there, and hope it adds to it's life, or to put it better...to add to the life of the 100bux you fork out for the single-purpose pressure cooker.

A teflon coated pressure cooker, with a pressure gauge and built in digital thermostat would bee perfect. Talk about cooking in style! Joy!

Working on a design to concentrate vinegar, using a hybrid between the setup at Orgsyn and a toaster .

It'll use 3 glass bottles, copper tubing, copper condensor to recycle acetone.
The nichrome wire can sit in the first glass where acetone drips, so that short circuiting isn't a problem.

ning
(acetaminophanatic)
06-17-04 21:16
No 514039




Actually
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If it in fact turns out that the limiting factor is only the boiling point of the alcohol, it might well bee the case that the reaction can be run in a reflux apparatus.

(the isopropanol/water azeotrope boils at ~80 C, ethanol+water ~78 C)

Hey, LWR ---- bees! What kind of temperature differential can you get from the bottom of the reaction vessel to the top of the refluxing solvent in the condenser? Greater than 15 degrees? Let's hear it!

Clandestine chemist // amateur pharmacologist

p2e3r4f5e6c7t8
(Hive Bee)
06-17-04 23:53
No 514066




Hey shane and all my other brothers in OZ.
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Hey shane and all my other brothers in OZ.
What the fuck do you mean that EtOh isent common in OZ eehheemmm, BULLSHIT, Look a little harder my freind.
And just one other question?, Why in another post hear do you say yoy want to concentrate vinegar, If its acetic acid your after then look a lil harder again because it sold as a crystaline salt in little canisters
If you do get stuck with it then PM me my OZ brotherand ill do what i can to help ya out as far as steering you in the right direction to find what your looking for

Ask no question's, and i will tell no lies.

Shane_Warne
(Hive Bee)
06-18-04 00:02
No 514068




I can't imagine they'll know.
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I can't imagine they'll know. Well I certainly don't.

I think you could bee right about a reflux being sufficient though, if the pressure is only required for a slightly higher temperature.

The only thing is, that everytime SWIM has used a ghetz condensor, even with a balloon, and H2S has been produced, it seems to come straight through the balloon.

Without a balloon it would reek. (even worse)

DrLucifer
(Hive Bee)
06-18-04 01:07
No 514073




Sorry guys, but it doesnt look like my sulphur
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Sorry guys, but it doesnt look like my sulphur is going to arrive today... Not happy Jan!!
Looks like swim can only play with styrene this weekend!
Over and out guys, swim will be under radar for a few days, possibly more, so in the meantime...take it sleazy!

I'm a diamond that is tired, of all the faces i've aquired.

wareami
(Hive Addict)
06-18-04 09:11
No 514125




Hmmmm
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Hey, LWR ---- bees! What kind of temperature differential can you get from the bottom of the reaction vessel to the top of the refluxing solvent in the condenser? Greater than 15 degrees? Let's hear it!

ning: I serious doubt that the temp would fluxuate 15?C from the bottom of the reactants (closest to heat source) to the reactant surface....
Since I've never measured the temp of those two points, I can't say for sure but would be surprised if even 10?C difference was recorded.
This of course would depend on size of rxn and vessel shape/size...ie...how deep the reactant pool.

Fighting for peace is like screwing for virginity.

geezmeister
(Of Counsel)
06-18-04 09:26
No 514127




top to bottom?
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I'm not sure of your question. If its whether there is a more than fifteen degree C difference between the flask contents and the temperature of the condensate at the point where it condenses inside the condenser the answer is yes. You can have that much difference in temperature bottom to top. The difference between the flask contents and the temperature of the bath the flask is in frequently exceeds 20C, and I assume a good part of that difference is the cooling effect of the condensed liquid dripping back into the flask.

mostly harmless

Shane_Warne
(Hive Bee)
06-18-04 16:26
No 514176




p2e3r4f5e6c7t8, your right, I haven't looked...
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p2e3r4f5e6c7t8, your right, I haven't looked very hard for EtOH, I could fractionally distill vodka, but I doubt Ill bother, as I think it will work with either 96% EtOH/4& pyridine or 96% EtOH/4% MeOH.

As for AcOH, it's good to learn new skills...Plus, if you read the post title, it states that what will bee discussed in the main, is P2P from polystyrene foam and acetone.

wareami
(Hive Addict)
06-18-04 17:21
No 514187




Yikes...
Bookmark Reply

Man that'll teach me not to reply to anything before I've had my coffee.
Sorry ning...I misread your question.
Geez musta had his coffee though cause his answer makes tons more sense than mine.
I'll be over standing in that corner!

Fighting for peace is like screwing for virginity.