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Rosco Bodine
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| Quote: | Originally posted by Matsumoto_Hideki
1# 250ml x .9849 = 246.225g
250ml x _____ = 156g (.624) - .0151= 60.89%
2# 450ml x.9849 = 393.96g
450ml x ____ = 350g (est) (.780) -.0151=76.49%
?? this right? |
The yield is a fraction expressed as a decimal equivalent , then read as a percentage . ( move decimal 2 places to the right to express answer as
percentage )
The numerator of the fraction is your actual actual dry weight of crystals in grams .
The denominator is the raw number of ( milliliters of acetone used ) , multiplied by .9849
Usually the denominator would be some weight in grams , but I have already adjusted the equation to be based on milliliters of acetone for convenience
, since it is a liquid volume measure .
For example , let's say you used 250 ml acetone and your end product was 175 grams of dried DPPP crystals .
You used 250 ml of acetone , so 100% yield would be 250 X .9849 = 246.225 grams DPPP
175 / 246.225 = .7107 = 71.07% yield
( based on acetone )
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Atom
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This may sound, stupid but are there any toxic gasses involved during the formation of diphorone?
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Swedish Chef
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Jome,
AP has several isomers, like the halfacetal CH3COH(OOH)CH3 (monomer) and cyclic acetal structures like [(CH3)2C(OO)]x, where x = 2 - 4.
On heating with catalytic amounts of Cupric salts in diluted HCl, AP and isomers are converted to aceton, H2O and O2.
AP and AP-isomers are (half)acetals of aceton and H2O2, while DPPP should only have peroxyether bonds (ROOR) which are not affected by Cu/H2O/H+.
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Matsumoto_Hideki
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thank you rosco
Ok, now one other thing I have been noticing about "DPPP" is that is doesn't react with metals very well unlike AP and others.
Anyone else see this?
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Mickhael
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Ok, after heating at 70c for another 6 hours or so, I have a dark green...semi-transparent fluid which is reasonably thick...which I assume contains
at least some amount of transformed Phorone...however should I continue heating until its even darker? I could detect no change from the dark green
even after a couple hours of more heating.
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Matsumoto_Hideki
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There is no green during the Phorone production
Hey, mike please see my webshots account here:
http://community.webshots.com/user/matsumoto_hideki
Please look a the photos as they will guide you through the steps of production.
--- Yes you keep heating the liquid until it becomes very dark red to almost black. Keep the reaction with a partially covered with a lid to keep the
acetone and HCl vapours recycling untill they have fully reacted.
The optimum colour of the liquid is Black and will not llet any light through. This Colouration must be obtained before you can start any
peroxidation.
**** TIP: DO THE FREEZING METHOD OF PEROXIDATION TO GET BEST RESULTS. IT IS ALSO A LOT SAFER!
[Edited on 4-1-2005 by Matsumoto_Hideki]
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Joeychemist
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Green! well that's great!
Hideki
Hold on there, pure phorone can be any color between yellow and dark green, so surly its precursors can be green?
How can you be so sure he's doing it wrong? I am actually interested to hear his findings and results. What did you do different then the rest of
us Mickhael? Just because you're reaction seems different from ours DOES NOT mean you have done it wrong, it may just actually provide us with
important information crucial to this thread, please share you're experiment results and conclusions in details
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Mickhael
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Ok, well heres what I did...
Sorry for deleting the previous post, it wouldn't let me add the file I wanted so just decided to repost rather then double post 
Maybe I wrecked the batch...but here's what happened:
I started out with aprox. 100ml 31.45% HCl and 100ml of acetone. The liquids were at room temp. and I put them in a 500ml flask, and heated that in
1/2" of water in a metal pot, to a temp. of about 70C, and held it there for 2 1/2 hours...without a cover on. In about 1 1/2 hours, there was a
loss of 100ml of liquid, and a transition from clear - yellow - orange - red, at which point it stopped changing over the course of the next hour. I
removed it from the heat and sat it on a shelf over-night, no change was observed except that I was down to about 75ml liquid by then. Upon hearing
that more heating was likely needed I proceeded to heat some more, at this point I put it back in the same pot, covered in saran wrap at the same 70c
and left it there for about 5 hours, it then changed to the dark green...which is semi-transparent, that happened in about 2 hours, and after that no
more changes could be observed, however when swirled it does exibit oily quailties (light oil) and light does pass through...but only as a lighter
haze...not like like through water clearness at all. I hope thats all the details...
I might try cooling the liquid and then adding the h2o2 tonight...what say?
Ps: Just as one of my first test videos, here is 3 drops of MEKP in a tiny christmas light bulb, ignited by a 12v battery.
[Edited on 5-1-2005 by Mickhael]
Attachment: !3 Drops of MEKP.wmv (612kB)
This file has been downloaded 1360 times
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mr.pyro
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Let me say, I have just tried the same procedure, with the phorone reaction covered.
I am slowly adding the H2O2 5 Ml at a time and this yield is amazing. It's not like a precipatate, its just like all the liquid in the beaker
transformed into DPPP, and I still have to add 150 more Ml of H2O2!! Ill post some pics and my synth later tonight.
[Edited on 5-1-2005 by mr.pyro]
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Matsumoto_Hideki
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Confusion Mickheal?
Alright, just to clear things up we are NOT making phorone here rather Phorone HCl which is DARK RED, Black oily liquid with a very punjent metallic
smell ... yes the initial stages of the reaction are yellowish idicating the acetone is changing to Phorone but the phorone produced becomes phorone
HCl in a matter of seconds while steeping the reaction at or near boiling point. (60-90c)
Mr. Pyroz I am glad you have discovered the high yeild DPPP synth produces. I
have got up 75-80% without trying too hard and a couple times 90% when the solution is completely concentrated.
By the way you should get at least 760g - 900g from a 1L jug of Phorone HCL.
Are you cold forming your DPPP in an Iceblock ?
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Joeychemist
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test the green stuff
Mickhael,
Yes please try to "peroxidize" the green solution, it could produce some very interesting results, or none.
Try cooling a few ml in a test tube and add H2O2 drop by drop until the reaction seems to stop, then right down everything you observe and report
you’re findings. You say you’re left with less than half of the original volume of the starting reactant chemicals, so I am wondering what exactly
you are left with???
Hideki, since you are reporting such LARGE yields, why not do some major blasting and testing to prove the VoD is 9000m/sec?
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mr.pyro
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Well I am not using any iceblocks, but I wrote up a little synthesis, and added some pics.
56k warning on the pics, they have big filesize.
http://24.251.195.35:1081/video/dppp%20synthesis.htm
Well I just updated this with more pics and final filteration. I got about 200g of DPPP out of this. This really is a great yeild and easy to make.
Now what to do with 200g of a sensitve primary?
[Edited on 5-1-2005 by mr.pyro]
[Edited on 5-1-2005 by mr.pyro]
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Pyroz
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Haven't weighed the material yet. I think the reaction gave something like 80% yeild--possiably more.
Hey--- I tested this material Mr.Pyro, and I have come to the following conclusion that 100 grams of DPPP will outdo a 250gram AP charge packed at the
same density.
Its so bloodly clear its scary!
[Edited on 5-1-2005 by Pyroz]
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Rosco Bodine
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I have some further information to share on my sealed bottle experiment involving slow heating 225ml acetone / 225 ml HCl for an extended period of
time . By the end of 96 hours the upper oily layer of yellow brown liquid which was slowly separating from the more reddish colored emulsion below ,
had grown in thickness to about 10 mm , but did not increase in volume during the next 24 hours so the heating was discontinued at the end of 5 days
of heating the mixture at 66 C .
The mixture was allowed to stand idle the sixth day without any heating . No further changes were observed on either day 5 of heating or day 6 as the
mixture was allowed to stand at room temperature .
The mixture has been transferred from the bottle to a jar sitting atop an efficient magnetic stirrer driving a rare earth stirbar and having
sufficient stirring capability for emulsifying viscous mixtures .
The stirrer was started and the mixture stirred rapidly to form an emulsion from the two liquid phases . Then to the rapidly stirred mixture at room
temperature was added in 5 ml portions every 5 minutes , 26.6% H2O2 . A moderate exotherm was observed and
the temperature held at 55 C during the
last two portions . Stirring was continued
for fifteen minutes and then stopped , the mixture allowed to cool . The phases separated , and the thickness of the upper oily layer was unchanged ,
but had taken on a greenish color . The lower reddish colored layer which had been opaque had clarified distinctly , now allowing a beam of light to
be seen passing through from the opposite side
of the glass jar , and having the same
dark red orange color of freshly brewed strong tea , as had been observed at about 6 hours into the beginning of the heating at 66 C , when it was in
the sealed bottle . So a transparency change is observed in the lower emulsion layer , in response to initial peroxidation at warm temperature ,
while the upper layer
has undergone a color change also , but
no change in volume . The mixture is allowed to stand for several hours and cools to 15 C .
The cooled mixture is stirred up to an emulsion once again and another 25 ml of H2O2 is added in portions . After the third portion is added , a fine
yellow precipitate is causing the color of the mixture to appear distinctly lighter so
the stirred mixture has the appearance of light brown paint , as opposed to the earlier near black color . Very slight exotherm is much less energetic
during these additions than during the earlier
additions . The precipitate increases as
each portion of peroxide is added .
After completing the additions of the second 25 ml H2O2 , the stirring is continued 10 minutes , and then stopped
and the mixture allowed to separate once more . The upper layer of oily liquid remains the same volume , and has a dark greenish color . The lower
reddish
layer has become even less darkly tinted
and is now a dark orange and has a layer
of light yellow colored preciptate on the bottom of the container . At this point it
is evident that the lower layer is more reactive and reacting preferentially with the H2O2 which is being introduced to
a stirred emulsion consisting of the upper oily layer and the lower "tea colored" layer . Unless the upper layer waits until
the lower layer is fully reacted , to begin
itself reacting , it is beginning to appear
that the upper layer may possibly be an undesired byproduct and not the same as
the phorone dihydrochloride in the "tea colored" layer below . Of course it is too early yet to be conclusive , because much more H2O2
remains yet to be added to see if the upper layer will diminish , but the early indication is that my earlier guess about the "cloud point"
marker for
the endpoint of the reaction producing the
phorone dihydrochloride may indeed be correct . If this should bear out , from my
rather tedious "slow motion" stepwise observations , it will be likely that the digestion of the initial acetone mixture has reached its
peak for the desired precursor , just before the oily surface
slick of a separate upper phase is observed . This oily upper layer could indeed be phorone , from the gradual
hydrolysis of phorone dihydrochloride already produced . And in this reaction
the appearance of phorone is undesired since it arises as a consequence of the decomposition of the precursor wished to be kept intact as the
dihydrochloride of phorone . So it appears that any excessive digestion of the initial mixture may decrease the yield . I will better be able to
confirm this with certainty after
completing the remaining additions of H2O2 . If the lower layer gets depleted and precipitation ceases , while the upper
layer resists peroxidation , then this hypothesis will be proved by my experiment . I will update concerning the finding when it becomes evident what
is the case .
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Joeychemist
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Very nice
Rosco, that’s exactly what we have all been waiting to hear, so it would appear that the top layer is waste material or worse our precious phorone
dihydrochloride that has decomposed from the extended heating period. But you mention the color change of the top layer as well, which indicates a
chemical change or reaction takes place somehow involving the top layer during the reaction.Hmmm, very peculiar.
Many more tests are needed to actually figure out what the top layer is and if it is important to the reaction. Another test where the top layer and
bottom layer are separated, then individually added to the H2O2 should produce some more tantalizing info and results.
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Pyroz
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interesting indeed...I wonder of pure DPPP is really yellow or that is some contamination of sorts. It would interesting to know.
[Edited on 5-1-2005 by Pyroz]
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Axt
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Do you have a density yet Pyroz? or at least a relative density to AP?
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Mickhael
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| Quote: | Originally posted by Matsumoto_Hideki
Alright, just to clear things up we are NOT making phorone here rather Phorone HCl which is DARK RED, Black oily liquid with a very punjent metallic
smell ... yes the initial stages of the reaction are yellowish idicating the acetone is changing to Phorone but the phorone produced becomes phorone
HCl in a matter of seconds while steeping the reaction at or near boiling point. (60-90c) |
I understand that, I'm just refering to it as Phorone for simplicities sake. I realize I probly don't have the desired product...but
I'm just trying things for the first time here. I think the most major difference with my attempt to make Phorone, is I let alot evaporate while
heating, so the reactions may not have had time to complete, because from what I've heard, in the 7 total hours I heated the liquid, it should
easily have turned to a thick black color in that time.
I'm currently cooling everything down outside, my Phorone is in an ice block...the temp. outside is currently -10c.
[Edited on 5-1-2005 by Mickhael]
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Rosco Bodine
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It is uncertain at this point that my hypothesis is correct . It could be that
as the lower layer is peroxidized that
the upper layer will begin to disperse
into the reaction zone , *if* the separated upper layer is the same material as the lower layer and was just driven out and
separated from oversaturation during formation . That would be okay too
because it would also reveal that you
can know when the precursor formation is finished when the upper layer stops growing . So the results will be useful information either way it goes .
But I have a feeling , just a guess really that
it is likely the decomposition product from
taking the digestion too far . There is a method to my madness the purpose of
which should be revealing itself . The emulsion which I am churning for this reaction makes the entire mixture look like milk chocolate during
peroxidation .
It is so well mixed it takes ten minutes to
stop swirling like smoke and even begin to stratify again , so the upper phase is getting every chance to redissolve and react further if it is going
to do that .
Presently I have 100 ml (~ 1/4 of the total ) peroxide
introduced , stopping and examining the
results after each 25 ml . It takes a couple of hours to get a read on what happened and resume . Mainly I am not trying to get a good yield of DPPP
, but to
see what the story is on the upper layer ,
whether or not it will enter the reaction .
Then obviously will be revealed a crucial piece of information which will define the
reaction endpoint determination for the precursor , so any subsequent synthesis aimed at producing the DPPP in a "clean" synthesis can be
studied for learning the other factors that likely also apply to increasing the yields , temperature and addition rates are two things likely to
affect the yields as well .
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Rosco Bodine
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| Quote: | Originally posted by Mickhael
I understand that, I'm just refering to it as Phorone for simplicities sake. |
You want simple ? Okay here's simple .
Actually , the most likely reaction scenario to me seems that first three acetones conjugate , stick together , polymerize to form * triacetone
dialcohol * ( a real compound that is something like a trimer of acetone ) It is similar to what happens with formaldehyde solutions when they
are acidified , the formaldehyde polymerizes to paraformaldehyde , an indefinite number polymer , or three formaldehydes can combine into a trimer?
(who knows!) called trioxane . The reactions of aldehydes and ketones are similar , so that fact lends support to my belief that the acetone
polymerizes to a trimer , triacetone dialcohol . Then it further enters a * condensation reaction * with 2 HCl's , with the
elimination of 2 H2O's , to form * phorone dihydrochloride * , which may be considered to be a
* derivative * of phorone because of structural similarity to phorone , while never requiring the formation of any phorone itself . Now
that's what I believe happens , and yeah it is different from what the patent says in words about "acetone polymerizing to phorone"
but hey here's the deal , phorone is not a polymer of acetone in anybody's book , if that book was written by anybody who knows the
difference between polymerization and condensation reactions . Sometimes one can follow the other like here . Condensation reactions are water
producers . And there is no way to get phorone from acetone without producing water . Anybody check me out on this please . So Mackowiak either
goofed or the word translation is inaccurate , however the symbolic diagram showing the reactions is aligned with what I am saying likely happens .
The 2 H2O's are sort of circled in bean shaped boxes on the * triacetone dialcohol *which is an acetone trimer . Even if phorone formed
as an intermediate , before then combining further with 2 HCl's , phorone would still be an acetone * condensation product * and *
NOT *any sort of " acetone polymer " BECAUSE acetone does not polymerize to phorone , but to diacetone alcohol ( the dimer )
, triacetone dialcohol ( the trimer ) , and even to higher polymers from what I understand may be possible , even to a solid plastic acetone polymer
.....none of which are ever phorone So the best phorone could ever be is a
* polymerization condensate * , a "dehydrated polymer" of acetone is another way of stating this .
I have gotten sick of the focus and emphasis on "phorone" like it is the precursor for its own derivative , when plainly if the reactions
are drawn correctly it is the dihydrochloride derivative of phorone which is the actual precursor .
Forget phorone ! Erase from your mind that DPPP comes from phorone !
DPPP no more comes from phorone than trinitrobenzoic acid comes from benzoic acid .
The structural similarity and similar names is where the similarity ends .
Cast out the phorone demon right now ! Save yourself from this "phorone illusion" ,
or I shall be forced to perform an exorcism to rid us of this pretender ,
this pseudoprecursor who deceives with subtlety and causes confusion
to the washer of test tubes and master of the molecular
This rant was brought you by reading and rereading the first stumbling half of this mammoth gargantuan thread one too many times
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Pyroz
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Your right--- I've fallen into the same trap a few times--- thanks for clearing the air and illuminating the "essence"
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Mickhael
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Alright, out with that word...
Well I firmly admit...Your smart, "i aint" lol, so what would you suggest we refer to when at the first stage of the synth?
"Dialcohol"? What is the appropriate term to save this thread from further confusion?
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Jome
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I have just completed the first phase of the reaction, and I'm about to evaporate excess water and acetone off.
But one thing strikes me a weird with my solution, its dark red as it's supposed to, but It has a HORRIBLE smell!
Smells metallic, and stings in the nose..... My sister wondered why I was experimenting with cat piss..... Could I have done something wrong? Only
thing I can think of is a possible iron contamination from the lid of the glass jam-jam I use.... (!?)
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Mickhael
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Results...if you can call them that :P
Jome...as far as I'm concerned the whole synth smells bad from start to finish...except perhaps the final product.
Now about my attempt to peroxidize my "green stuff" That was a complete flop...I cooled everything, and slowly 10ml at a time, added twice
the h2o2...and absolutly nothing happened...so just in case I added 5ml of the same HCl as before...nothing. The only change of any kind was when I
decided to add the bi-carb to be safe and the damn thing fuzzed and bubbled over the top. So whatever it was i made, it isn't the right thing for
DPPP! I must have allowed to much to evaporate, and the reactions never finished properly to allow the correct precurser.
Of somewhat enteresting note however, I have started heating another batch of Acetone and HCl in the same flask as before, and there was a small bit
of black residue left inside it, which I left because I figured I was working with the same ingredients so why not?
Anyway, I began the heating again, except this time slightly higher...at 75c...and in a larger batch of 400ml total (covered of course) Now withen
just 20 minutes and no noticeable bubbling as with the last time...the whole container has changed from clear to dark red! The change was so fast in
fact that it was almost straight to red before I walked back in the kitchen and noticed. So maybe its possible to seed the reaction, and get it
started faster by having a little of previous batches in the new one?? Hmm.
1 Hour after applying the heat...(now staying around 80c) and the mixture is completely black! With no trace of red even when held up to a bright
light. I think this 'seeding' idea might have some merit...anyone else have experience with this?
2 hours, 10 minutes - removed from heat and sat on a shelf uncovered, at 21c for the night, liquid is now thick, oily and very black! Woo, I think
I've got it this time
[Edited on 5-1-2005 by Mickhael]
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Rosco Bodine
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| Quote: | Originally posted by Mickhael
Well I firmly admit...Your smart, "i aint" lol, |
Oh not so smart really , because I was buying into
the original premise just like everyone else for a long time and that was preventing any arrival at a "working knowledge" of the reaction
being realized. | Quote: | | so what would you suggest we refer to when at the first stage of the synth? "Dialcohol"? What is the appropriate term to save this thread
from further confusion? |
Maybe acronyms are best to save typing of long names of compounds . Perhaps for " triacetone dialcohol " we could call it TADA , and for
" phorone dihydrochloride " we could call that PDH or PDHCL ? . For the " pentachlorophorone " perhaps call that PCP eek !
, or maybe PCPH ? Acronyms aren't my talent . Maybe a military guy around here will give these precursors proper acronym nicknames .
Anyway , to update on my experiment , it looks pretty conclusive that the "black oil" which floats to the top ond forms a slick or a thicker
upper layer gradually is NOT the desired precursor , but is likely a decomposition product of the precursor .
Efforts at peroxidation of an emulsified mixture of the upper layer with the lower layer have resulted only in reaction of the lower layer , and even
worse it appears that the material of the upper layer causes decomposition of the end product upon extended contact with the precipitated DPPP in the
stirred peroxidation mixture . So I believe at this point I can safely declare you do NOT want the "black oil"
or "yellowish brown oil" which separates from the "dark red orange" product which forms first . These are evidently two entirely
different substances which form when the mixture of acetone and HCl is digested . Now it could well be true that
heating aggravates the production of the undesired "black oil" , and that simply letting the mixture of acetone and HCl sit and digest
slowly at room temperature for
an extended time will give more of the desired "dark red orange" tinted material .
This has not been tested so far as I remember . But it would seem to be a plan as an alternative to the more accellerated digestion reaction at 66 C
which would complete in something about 6 hours , if the obseved reaction repeats
closely with slightly increased HCl which may change the time . My next experiment will likely involve the same sealed bottle approach except with
the digestion being stopped at the "cloud point" where the dark colored mixture loses its clarity to a strong light , and begins to become
translucent . This should result in a cleaner synthesis mixture , whatever may be the subsequent conditions for peroxidation .
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