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Author: Subject: Diphoronepentaperoxide (DPPP)
Chris The Great
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[*] posted on 29-1-2005 at 00:21


How hot did you get the HCl? I certainly would hesitate to heat my HCl as it fumes alot already when it's cold....

Can you give more deatils (ie Exactly what you did)?

Even if phorone is formed, keep in mind that it will not form DPPP by being peroxydized.
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[*] posted on 29-1-2005 at 10:43


OMG why do you people keep asking the same question when it's been answered 20 times???? Thats why this thread is so long
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Matsumoto_Hideki
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mad.gif posted on 29-1-2005 at 14:09
YES I KNEW Phorone is a DEAD end


HCl was heated to 100c.

Some people are claiming that 1:1 concentrated HCl to acetone does not produce phorone but it is, obviously as there are byproducts being coproduced ie) mesityl oxide.
and mesitylene. I think the problem is that we are not adding enough HCl to get the pentachlorophorone.
Instead we may be geting a trimer or a dimer of Chlorophorone leading to a triperoxide version of the synth? I am very sure that we are not getting a mesityl peroxide..
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[*] posted on 29-1-2005 at 14:26


I've said this before over at E&W, and you called me an immoral person, but it is coming true. Evidence is coming out against you, and you refuse to accept it. You keep going on with your stuff and basically ignore the mounting evidence against your compound. I said that you would never want to give it up, because you want this discovery associated with you.
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 14:45
Antisocialite Painkilla


Evidence is mounting up against you painfull.

Could you please look at the chemsynth website before posting about the production of mesityl oxide. There is a great BIG synth regarding the action of HCl on acetone. This idicates that mostly phorone and phorone derivatives are in fact the main products instead of mesityl oxide.

DON'T FLAME ME DUDE OR YOU'LL WEAR IT! And don't use the messaging on this page to flame me either!!
]:mad::mad::mad::mad:

[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 15:15
CHEMSYNTH WEBSITE


Read what others have posted painfull.
CHEMSYNTH WEBSITE
look up mesityl oxide and you will see the light.
WTF with name calling you immature little shit!

[Edited on 29-1-2005 by Matsumoto_Hideki]:mad::mad::mad::mad::mad::mad::mad::mad:

[Edited on 29-1-2005 by Matsumoto_Hideki]
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 15:21
READ THIS PAINFULL


There are two general methods for the preparation of mesityl oxide: the action of condensing agents (hydrochloric acid, etc.) on acetone, 1 and the dehydration of diacetone alcohol. 2 The action of acid condensing agents ]is very unsatisfactory; the yields are poor and considerable quantities of phorone and similar substances are invariably produced.

from "Organic Syntheses, Coll. Vol. 1, p.345; Vol. 1, p.53"

other sources
Fitting, Ann. 110, 32 (1859); Heintz, Ann. 178, 343 (1875); Claisen, Ann. 180, 4 (1875); Freer and Lachmann, Am. Chem. J. 19, 887 (1897); Currie, J. Am. Chem. Soc. 35, 1061 (1913); Couturier and Meunier, Compt. rend. 140, 721 (1905); Mannich and Hâncu, Ber. 41, 574 (1908); Bodroux and Taboury, Bull. soc. chim. (4) 3, 829 (1908); Yllner, Svensk. Kem. Tids. 37, 227 (1925) [C. A. 20, 739 (1926)]; Gasopoulos, Ber. 59, 2188 (1926); Brederick, Lehmann, Schönfeld, and Fritsche, Ber. 72, 1417 (1939).


Heintz, Ann. 178, 351 (1875); Kohn, Monatsh. 34, 779 (1913), Ger. pat. 208,635 [Frdl. 9, 62 (1908–10)]; Kyriakides, J. Am. Chem. Soc. 36, 534 (1914); Hibbert, ibid. 37, 1748 (1915); Hoffman, U. S. pat. 1,474,035 [C. A. 18, 401 (1924)]; Locquin, Ann. chim. (9) 19, 32 (1923).
Hoffman, J. Am. Chem. Soc. 31, 722 (1909); Hertkorn, Ger. pat. 258,057 [Frdl. 11, 46 (1912–14)].



[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 15:40
getting back on track to DPPP


Lets get back to planet earth shall we. Chemsyth has stated that phorone comes from HCl on acetone along with mesityl oxide as a MINOR co-product. i am sure we have a phorone peroxide but i also beleive that we need to add more HCl to the solution. I think this is going to lead us to our product.
I really pitty those people who can't read a chemsyth report.:P
BTW speaking of spelling, "foick" should be written fuck. hence in the verb "to fuck" or to be "fuck out of luck" example: painkilla was fuck out of luck when it came to reading.


There are two general methods for the preparation of mesityl oxide: the action of condensing agents (hydrochloric acid, etc.) on acetone, 1 and the dehydration of diacetone alcohol. 2 The action of acid condensing agents ]is very unsatisfactory; the yields are poor and considerable quantities of phorone and similar substances are invariably produced.

from "Organic Syntheses, Coll. Vol. 1, p.345; Vol. 1, p.53"

other sources
Fitting, Ann. 110, 32 (1859); Heintz, Ann. 178, 343 (1875); Claisen, Ann. 180, 4 (1875); Freer and Lachmann, Am. Chem. J. 19, 887 (1897); Currie, J. Am. Chem. Soc. 35, 1061 (1913); Couturier and Meunier, Compt. rend. 140, 721 (1905); Mannich and Hâncu, Ber. 41, 574 (1908); Bodroux and Taboury, Bull. soc. chim. (4) 3, 829 (1908); Yllner, Svensk. Kem. Tids. 37, 227 (1925) [C. A. 20, 739 (1926)]; Gasopoulos, Ber. 59, 2188 (1926); Brederick, Lehmann, Schönfeld, and Fritsche, Ber. 72, 1417 (1939).


Heintz, Ann. 178, 351 (1875); Kohn, Monatsh. 34, 779 (1913), Ger. pat. 208,635 [Frdl. 9, 62 (1908–10)]; Kyriakides, J. Am. Chem. Soc. 36, 534 (1914); Hibbert, ibid. 37, 1748 (1915); Hoffman, U. S. pat. 1,474,035 [C. A. 18, 401 (1924)]; Locquin, Ann. chim. (9) 19, 32 (1923).
Hoffman, J. Am. Chem. Soc. 31, 722 (1909); Hertkorn, Ger. pat. 258,057 [Frdl. 11, 46 (1912–14)].





[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]

[Edited on 29-1-2005 by Matsumoto_Hideki]
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 15:53
Can u prove this?


Ahh, but you missed one point in that when the H2O2 is added to the PCP we have chlorine being released from the solution. In all my synths this was the case. I think most people have smelled this during their reaction as well.

[Edited on 29-1-2005 by Matsumoto_Hideki]
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Matsumoto_Hideki
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[*] posted on 29-1-2005 at 16:00
Chlorine is destinct as a smell


well the gas coming from the reaction, besides smelling like chlorine it also acts like chlorine by making white ammonium chloride fumes apon expose to ammonia vapour. well duh it is chlorine. This chlorine is obviouly being used as it is being ejected when the CP is being peroxidized.

BTW spelling helps to. chlroine is Chlorine :P



[Edited on 30-1-2005 by Matsumoto_Hideki]
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[*] posted on 29-1-2005 at 16:13
Stop this now!


I am sick of this flame war. Hideki shut up!

I try to Ignore him, as should everyone else. you are acting like children rather then a matured adult capable of conducting a civilized factual conversation. This thread and the content have deteriorated due to flaming, bullshit and a complete lack of common sense.

What’s next, will you guys be reverting to primates? Will you then throw feces at each other as well?:mad:

Stop it now!:mad::mad:

I would now ask for a moderator to step in, as this has got to stop. Moderators I’m not telling anyone how to do there job, but you do have a job to do, you agreed to keep the forum in order and protect it from disruptions and flame wars. Please, please discipline and order are needed.
:(;)



[Edited on 30-1-2005 by Joeychemist]
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[*] posted on 29-1-2005 at 16:28


I've warned you guys, about 10 pages back I guess, about nutcases like Hideki. But who would listen?

This is what you get for allowing idiots to roam around freely.

This moron is even rude enough to send me reports about other people flaming him, go figure.

I hope you've all learned your lesson.

Hideki has been BANNED.




One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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[*] posted on 29-1-2005 at 16:34
residual peroxide experiment crystallizing now


Earlier today I repeated my synthesis using the method which before produced a nearly quantitative yield of 98 grams of alleged DPPP from a precursor made from 100 ml acetone . And three hours later ,
after the formation of the alleged DPPP , I added 100 ml acetone gradually which caused to temperature to rise again from the - 2 C to 10 C , indication some further reaction is occurring with what is believed to be unreacted peroxide from the DPPP reaction . The ice bath has been refilled and the stirring continued and the batch has been running now for 5 hours since the beginning . The mixture will be allowed to stir at least another 4 hours and then will be left to stand overnight in the melting ice . In a couple of days , perhaps three , I should have a dry weight for the product of this reaction .
The weight of this supposedly "mixed product" derived from a total of 200 ml acetone and 280 ml 27% H2O2 should provide some useful information . Because the peroxide should have been depleted in reaction with the 100 ml of acetone in the precursor if DPPP was produced , and the total theoretical yield possible for that 100 ml acetone converted completely to DPPP would be about 98.5 grams of DPPP . Adding a second 100 ml portion of acetone to the
"spent" DPPP reaction mixture should therefore not result in much of an increase in the weight of any "mixed product" of AP with mostly DPPP already produced , *if* the first product actually was DPPP . If I end up with some much greater amount than 100 grams or so of dried product from the acetone treated "spent DPPP reaction mixture" . then the entire theory for the supposed chlorination route to DPPP is in some serious trouble because of the stoichiometric impossibility presented by
unreacted residual peroxide sufficient for forming an added amount of ordinary AP from the mixture where the peroxide should have been already spent .
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[*] posted on 29-1-2005 at 16:44


I thought the theory with chlorination has been disproved already? Will someone neutralize thier mixture because I am getting some interesting results (i mean nuetralize the precursor mxiture the dark red one)



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[*] posted on 29-1-2005 at 17:14


Quote:
Originally posted by PainKilla
I thought the theory with chlorination has been disproved already?
Nope the chlorination theory has not been disproven before , but my residual peroxide experiment has the ability to do just that , and more . That is precisely why I am doing the residual peroxide experiment , it is good information provider .
Quote:
Will someone neutralize thier mixture because I am getting some interesting results (i mean nuetralize the precursor mxiture the dark red one)
This was already done in the early part of the thread , and repeated later . I do not see what pertinent information is revealed , or what is the purpose for neutralizing the precursor . I can however see what is the relevance of unreacted peroxide in a "DPPP" spent reaction mixture , when that unreacted peroxide shouldn't be there .
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[*] posted on 29-1-2005 at 17:15


If I made something using H2SO4 then no Cl is nessacary, therefore disproven....

[Edited on 30-1-2005 by PainKilla]




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[*] posted on 29-1-2005 at 17:29


Quote:
Originally posted by PainKilla
If I made something using H2SO4 then no Cl is nessacary, therefore disproven....
Wouldn't you need to know what the "something" you made actually is , or at least if it is exactly the same product as produced using HCl , having the same consumption of H2O2 involved in the formation of your "something" , in order to conclude that chlorination is disproven ?
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[*] posted on 29-1-2005 at 17:37


I did everything the same as the HCl method jsut replaced the acids.... It wil be filtered soon but everything looks *exactly* the same.



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[*] posted on 29-1-2005 at 17:54


Painkilla, as I tried to explain to you over U2U, physical properties are not the same as chemical properties, therefore you can not possibly claim that it is or isn't the same reaction occurring as you have not even collected or tested the precipitate. ;)
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[*] posted on 29-1-2005 at 18:04


Interesting , but it really doesn't prove anything so far except that you get a product which looks the same by substituting sulfuric acid for hydrochloric acid . Do you follow what I'm saying ? It is not a useless experiment . However, it doesn't get at the *heart* of the patents described course of reaction for DPPP by way of chlorinated intermediates , the chlorine for which is provided by the consumption of hydrogen peroxide in reaction with HCl . The level of H2O2 in the spent DPPP reaction mixture is therefore a critical evidence for or against the patents claim for the course of formation of the DPPP . If the residual levels of H2O2 in the spent DPPP reaction mixture do not reconcile with the amount of alleged DPPP product obtained , then the course for the reaction is different or the product is not DPPP , because the numbers don't add up . And in chemistry the numbers have to add up .
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[*] posted on 29-1-2005 at 21:23
I Hate you murphy, hate you so much....


Ok, well, I have a few days off school as finals are over for me, but not for others, so no school until next thursday. So, I figured I try to do some experimentation myself.

First, I decided that I will try several routes to the precursor, using different acids; hydrochloric, sulfuric and sodium bisulfate. I would then try to see if the same product was formed by testing each produced peroxide extensivly to either prove or disprove PainKilla's theory.

So, I got out some jars, cleared my very messy lab, and starting working. First, I measured out ~115mL acetone into each jar.
Then, 105mL 32% HCl was added to the jar with the plastic lid (plastic won't be attacked by the HCl fumes). It heated up and maintained a nice warm temp. I set it aside and measure out some 97% sulfuric acid (60mL) and 300 grams of solid toilet bowl cleaner (40% sodium bisulfate....work with what you have :P ).

http://img199.exs.cx/my.php?loc=img199&image=0016sk.jpg

I figure I can afford to lose some of my hard to get sulfuric as it's going to help us understand this mystery....so I thought :mad:

Well, this is about where things got really really bad and murphies law basically....pissed me off.

I slowly poured the sulfuric acid into the acetone to be greeted by the acetone exploding out of the jar in a blast of acetone vapour, somewhat like pouring hot acid onto a carbonate. I rushed to clean the acid/acetone of my hand and digital camera, and succeeded somewhat, although I had to pour water all over my hand as it had started to burn.

The mix, after reacting for 20 seconds had turned a nice, deep ruby red and was boiling quite nicely.

http://img199.exs.cx/my.php?loc=img199&image=0026sx.jpg

Well, that was nice, except another 20 seconds later it was deep black and still boiling.

http://img199.exs.cx/my.php?loc=img199&image=0036kv.jpg

Time to clean this up and cap this. So, I put on my rubber gloves and.....spilled the shit all over my bench! The jar was slippery as hell because of all the acetone!

http://img199.exs.cx/my.php?loc=img199&image=0046mo.jpg

This is where my messyness worked against me. Usually I will clean my bench up very good if I'm going to do somethign dangerous, but this was supposed to be a slow reaction that requires hours to complete with heating!
The stuff was horrible to clean up, it got everywhere. I stuffed paper towels underneath the crack between the thick boards that made my table, to keep it from puddling on my microwave, and spent 15 minutes cleaning this stuff up. About this time the reaction had finished, and it smelt AWEFUL. Bad enough I felt sick. But I had to keep cleaning.

I then decided to put the jar outside since it was really smelling bad and white fumes where coming off it. I spilled it again, this time it was really thick and foamy. AAUUGGHH. This spill was smaller though, since it was thicker. But it smelt HORRIBLE.

The next 20 minutes involved me taking all the stuff out from under my bench, wiping tons of this stuff off it, feeling sick to the stomach and getting really mad as the experiment was ruined.

In the end, I got a nicely stained workbench. Someday this thing is just going to explode from all the built up chemicals in it.

http://img199.exs.cx/my.php?loc=img199&image=0058yr.jpg

I left the pile of toilet cleaner next to it to help counter the horrible smell.

I'll try the stuff again tommorrow, and maybe do the sulfuric acid reaction again in a big jar so it doesn't boil over and make a video of it....it WAS pretty cool except for it getting everywhere and making me feel sick....

Sorry for ranting here, but hopefully someone can learn from my really bad luck.

EDIT: Heh, I just noticed that the 4th picture kinda looks like blood sprayed out of my face all over my experiment :P

[Edited on 30-1-2005 by Chris The Great]
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[*] posted on 29-1-2005 at 23:46


Please pardon me, guys. I have been reading through this thread for some time trying to make heads or tails of it, but I must thank the person who made it now able to be read from Matsumoto's last post on out. Though I offer no valuable contribution to this thread, I must say this:

Thank you, Vulture, for putting a stop to Matsumoto/Mr. Anfo/whatever he will be next week. I mostly frequent the E+W Forum due to their compatablity with weapons (which I am more prolific with), but I do many times enjoy your forum here, though, and am glad to see "Mr. Asian Polymorph" go bye bye. He has insistantly spewed his falsities at E+W with posts about how HIS DPPP detonates at 9000 mps (regardless of actual proof) in more than one thread. I'd be willing to bet he's not roomies with J-Scan other than in his head (or pants, your guess).

Mumbles was right. But now that Matsumoto is banned here we have to hear his insistance moreso over there, I speculate.

If I might be so bold as to offer a bit of advice: If it's possible to do an IP ban on Mr. Matsumoto, do it now, and be done with the whole bunch of personas in his head. Rogue Science will sick of him soon and do the same.

There is no LAN. They are all one and the same.

I'll retire to my place in the shadows to learn, now. (AHEM, who do I return the soapbox to?).
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[*] posted on 30-1-2005 at 07:48


I have read this entire topic, over and over. I have also talked to people here in sweden, I have read other pages too. DPPP is almost sulphur coloured fine powder. I have tried to make it. First time i got white powder, 2nd time grey, and the final time skin coloured. What am I doing wrong? My powder is finer than AP and has another colour, but it smells like AP and has the wrong colour. Has anyone here made it and succead? And if, could he/she pleas explain exactly how?

P.S. Excuse my bad english, hope you at least understand what I mean .

[Edited on 30-1-2005 by Obersturmführer]




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Rosco Bodine
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[*] posted on 30-1-2005 at 09:24
"mixed" product from residual peroxide experiment


The product obtained from my experiment has been filtered and is drying . Of course I will have no actual weight until the product has finished drying , but from the volume of the crystals it is plainly evident there is a massive increase in the "mixed product" obtained by adding a second portion of acetone to the supposedly "spent" DPPP reaction mixture . As a strictly visual estimate there appears to be at least a 50% increase in the product and perhaps a 75% increase or even more . I can't tell for sure how much until the productt is dried . But just from what I am seeing as a result from this experiment , the entire matter of the DPPP as a composition of matter obtained by the route specified by the Mackowiak patent is in serious doubt because of the evidence of unreacted peroxide in the DPPP reaction mixture , in
an amount that makes the reaction scheme specified by Mackowiak *impossible* . The dry weight of the "mixed product" will likely shed some further light upon what is the probable material which we have alleged is DPPP .
At this point it would surprise me none at all if the supposed "DPPP" turns out to be nothing more complicated than a variant of AP , or something very close to AP , if not indeed simply AP which has been "tinted" slightly by some polymerized acetone impurity . Can everyone almost hear Axt chuckling at this point , saying uh huh I told you so ?
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[*] posted on 30-1-2005 at 09:50


Lol, that is what I said too, but nooone lsitens. I am going to filter out my stuff later today hopefully. Also of interest is this:

Acetone with NaOH, makes the same yellow color!

Puzzling eh?




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