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Mastermind
(Stranger)
06-18-00 10:28
No 18563
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P2P 
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Anyone ever see one of these bottles.
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Mastermind
(Stranger)
06-18-00 10:32
No 18564
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Re:
P2P
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It really helped FOAF develop his skills with this type of chemistry.
FOAFOAF got three bottles for him around 20 years ago. More pics to
come (ie. chems used to make p2p, etc.). Stay tuned. Lots of
tips, too.
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Rhodium
(Chief Bee)
06-18-00 10:48
No 18569
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Re:
P2P
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Wonderful! I want one of those, I want one of those! (empty is all right).
http://rhodium.lycaeum.org/
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Mastermind
(Stranger)
06-19-00 15:00
No 19044
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Re:
P2P
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Here's some more pics. Ten bottles of benzyl chloride and 5 lbs of
NaCN. FOAF had 5 lbs of PAA at one time but all he has left is an IR
spectrum. FOAF'll get the references together and tell what he thinks
is the best processes (that he tried).
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obituary
(Hive Bee)
06-19-00 21:36
No 19192
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Re:
P2P
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swim has access to a broader range or a little more common chemicals of less
proportions and is very envious. esp. the phenyl compouns, the BzCl is
nice too esp in that quantity- all swim has to say is damn your good luck
good lunch
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Mastermind
(Stranger)
07-01-00 19:55
No 23789
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Re:
P2P
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I've been busy and couldn't get back sooner. So maybe I'll post a
little at a time (looks like I'm on a roll here so I'll keep going; edited 3
hrs later). FOAF discovered after much experience with the acetic
anhydride process and the Thoria tube furnace reaction (Organic Synthesis Vol
2 pages 389-391) that the magnesia tube furnace he developed on his first try
was the holy grail of P2P, in his opinion (assuming you have PAA). This
was discussed by someone using the username OTC on the old Hive board
(talking to oilman and I think CHEMMAN; others seem to know about the tube
furmace,too). The rest of the references are:
Vogels mentioned here a lot, and
US patents:
2108156
2612524
2697729
2811559
3075016
3660491
4172097
4754074
5750795
You can download these patents from http://www.micropat.com/
Patents issued in 1976 and later can be viewed at the IBM (I think) and USPTO
web sites.
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Mastermind
(Stranger)
07-01-00 20:15
No 23792
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Re:
P2P
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The magnesia catalyst was made using pea sized pumice (some patents were seen
supporting similar catalytic materials using perlite for cracking petroleum
hydrocarbons; other art). Enough pea sized pumice to fill FOAF's
combustion (now catalyst) tube was covered with enough Milk of Magnesia so
that the pumice 'had looked like it had been white washed' (good description)
and at the same time the pores were not clogged (for maximum catalytic
surface area). A 98% silica combustion tube was used which was wrapped
with a heating tape (max temp 800 degrees C) and was covered with glass wool
as insulation. 2-3 teaspoons of calamine lotion (ZnO and Fe oxide; see
US patent 5750795, for example, especially tables 1 and 2) was added to the
catalyst and it was heated, alternately, on a gas stove and in a microwave
oven to dry it and convert it to MgO. It was found that when the
catalyst was placed in the tube and heated to about 500+ degrees C (with air
pumped through it) that the Mg(OH)2 could more easily be dehydrated (H2O
given off and condensed) and converted to MgO.
*Note: add calamine lotion before putting in combustion tube (maybe a little
sloppy here, have to read over it some more, questions must be in chemical
language as formally taught in college, nothing else will be understood (I
did get a couple private messages))
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Mastermind
(Stranger)
07-01-00 20:34
No 23796
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Re:
P2P
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A mixture of PAA and acetic acid was passed through the tube at around
400-450 C (see the Organic Synthesis article for setup of the apparatus;
heating tape used in place of the electric furnace). An aqueous layer
and organic layer was obtained (smelled sweet like P2P and maybe a little
like burnt rubber, too). The next night some Mn carbonate (see Vogels,
etc) was added to the rest (last half) of the PAA and acetic acid, as well as
some being placed in the tube (no effervesence was seen from the Mn
carbonate; see also US patent 4754074 which uses decomposable Mn salts, such
as the acetate). The process was continued and it was found that after
the addition of the Mn carbonate that the product smelled a lot sweeter like
pure P2P (see bottle above). The organic layer was washed with NaHCO3
solution, centrifuged using an old centrifuge bought for $18 in an antique
store to seperate the emulsion, distilled at atmospheric pressure to check
its boiling range (good range) and reacted with formamide in the Leukart
reation to get the amine in good yield. The aqueous layers mentioned
above should be extracted with solvent to recover more ketone.
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Mastermind
(Stranger)
07-01-00 21:08
No 23810
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Re:
P2P
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Its well known that phenylacetonitrile (refered to here as PAN) can be made
from benzyl chloride (BzCl) and NaCN. FOAF found that when trying to
distill PAN under a vacuum according the Organic Synthesis article (another
article on PAN from BzCl and NaCN) it bumped so badly that it was almost
impossible to do, even using a distilling column and claisen adapter.
The use of a capillary tube leading into the distilling flask was not
tried. Later, FOAF realized he could probably distill it at atmospheric
pressure and tried it. It worked very well and the PAN distilled in a
narrow 10-12 degree range without bumping (most of it distilled at around 208
C, I think, which is its boiling point, ie. at least 95% distilled at this
temperature. It was found that if a clear distillate is obtained
(smells something like BzCl except less pungent and more cinnamon-like) and
hydrolyzed with dilute H2SO4 according to another Organic Synthesis article
that the resulting PAA comes out off white or yellow and can be used in the
tube furnace without purifying it by vacuum distillation.
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Mastermind
(Stranger)
07-01-00 21:56
No 23826
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Re:
P2P
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Now getting to the PAA. As is known it melts at about 77 C. The
Organic Synthesis article that describes its synthesis from PAN includes
vacuum distillation in its purification. FOAF found this to be
impractical since it seems to boil at such a high temperature, as well as the
fact that the constant sound of his vacuum pump drives him nuts
sometimes. So he decided that going with freshly distilled (at 1 atm)
PAN for making PAA is the best way, and not distilling the PAA for use in the
tube furnace.
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Mastermind
(Stranger)
07-01-00 22:10
No 23830
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Re:
P2P
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Also, for some reason, FOAF found that when he tried to hydrolyze the PAN
with dilute H2SO4 (according to Organic Synthesis) for some reason it would
not solidify when cooled (mp of PAA is 77 C). He thought about this,
visualized the triple bond between the C and N and decided to try adding
HCl. It worked. The organic layer above the aqueous layer
solidified when cooled. Later, FOAF read in a chemistry book in the
library that HCl works better when hydrolyzing nitriles compared to H2SO4.
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Mastermind
(Stranger)
07-01-00 22:23
No 23831
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Re:
P2P
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Conclusions: After years of experimentation FOAF finally decided that
maybe it is true that some of the most respected publications in chemistry
don't necessarily have the best syntheses.
For example, he found that the magnesia tube furnace (it is patented, by the
way) is superior to both the acetic anhydride process and the thoria tube
furnace reaction in Organic Synthesis. Also, distilling PAN at atm P is
better than distilling under a vacuum and using HCl is better than H2SO4 when
hydrolyzing PAN. The Organic Synthesis article also mentions in the
notes the use of a mixture of acetic acid and I think HCl and H2SO4, for
small scale production, which gives a yield of about 100%. My
xerox copies are a mess.
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Mastermind
(Stranger)
07-01-00 22:35
No 23835
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Re:
P2P
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FOAF developed these techniques for 15+ years without the knowledge of the
I2/RP process discussed here (other forums) and was surprised when he found
out about the extensive use of pfed. The experience gained here might
be best applied to other analogs or if the precursors are easily available or
if pfed becomes restricted, the techniques described here could be used.
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Mastermind
(Stranger)
07-01-00 22:47
No 23841
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Re:
P2P
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The process(es) described above is/are probably the most well known or
"industrial" process(es). It definitely facilitates large
scale production.
-------------
posts made possible by phenethylamines
everything in moderation
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oilman
(Newbee)
07-02-00 02:11
No 23873
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Re:
P2P
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Well mastermind,I'm fuckin astonished at the info that you have presented.I
too have all available chems to dream this method and I can say that the
route that you prescribe is the exact same route which I researched years ago
before there was such a thing as the hive.I am currently dreamin the seudo
way and plan on dustin the ol' bottles from the shelf to go the tube furnac
route.Your thread here is of great value to me ,especially since I have 200l
of benzyl chloride available(yes thats right!!).Thanks for the insight to my
future dreams
Oilman
I take my hat off to ya !!
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Osmium
(Moderator)
07-03-00 02:12
No 24197
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Re:
P2P
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I think this post should be moved to the chemistry or serious chemistry
forum.
Please give a more detailed writeup. I'm sure Rhodium will post it at his
site.
This really needs more discussion (which it will not get here in the newbee
board).
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Mastermind
(Stranger)
07-03-00 03:36
No 24218
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Re:
P2P
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Another thing I should mention is to keep a bucket of ice water around when
making PAN from BzCl and NaCN. The reaction is exothermic but not as
bad as the Grignard reaction. If it starts heating up too much by
itself stop stirring and put the reaction flask in the bucket of ice water
just like you would do to control a Grignard reaction. The reaction
slows down a lot after about 3 hours. Its best to stir it for about 8
hrs, too, to make sure the reaction is complete.
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oilman
(Newbee)
07-03-00 05:04
No 24239
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Re:
P2P
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The conversion of benzyl chloride to benzyl cyanide was quite a simple
process for me except that it should be done with extereme care(fume
cupboard!!,gloves etc).I have about a pound of NaCN left so I intend on doin
the conversion in time.I have been an advocate of the tube furnace since I
realised this method but it doesn't seem to catch on to well.By the way my
first experience with NaCN kinda had me staggering out of the room with
numbness creeping up to me and bloodshot eyes,quite an experience I will
never forget!!
I also have crude PAN stored in a container(kept in the dark).Would you know
the shelf life of this product.
Also do you have experience in Grignard to PAA??
Oilman
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Mastermind
(Stranger)
07-03-00 17:51
No 24433
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Re:
P2P
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OK, Osmium. I'll look into doing that. It might be a little
tricky writing up the process without a drawing of the apparatus,
though. If you look at both the Organic Synthesis article and in Vogels
you'll notice that they both have drawings of tube furnaces. This seems
to be necessary since it isn't a commonly used setup. I found one thing
on Rhodium's site that has a drawing; the aspirator pump. If a drawing
isn't possible, then I'll have to think about how to describe the apparatus
and how it's setup as well as the process.
I was just at the library today to check the volume numbers. The three
Organic Synthesis articles refered to here are:
Benzyl Cyanide, Organic Synthesis Collective vol. I pg. 107-109 (from benzyl
chloride and sodium cyanide)
Phenyl Acetic Acid, Organic Synthesis Collective vol. I pg. 436-438 (by
hydrolysis of benzyl cyanide)
Methyl Benzyl Ketone, Organic Synthesis Collective vol. II pg 389-391 (from
phenyl acetic acid and acetic acid using the tube furnace method with thoria
catalyst on pea sized pumice)
Note: Benzyl cyanide is also known as phenylacetonitrile (the nitrile
theoretically from phenyl acetic acid) and methyl benzyl ketone is also known
as phenyl-2-propanone (P2P) or phenyl acetone.
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Mastermind
(Stranger)
07-04-00 08:57
No 24655
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Re:
P2P
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Oilman, I sent you a private message. Some more tips I can think of are
the need for glasswool and a buchner funnel when filtering out the NaCl when
making PAN (benzyl cyanide). Filter paper tends to clog up. Also I
recommend weighing out the NaCN in a large oil pan that will hold the NaCN
bottle and scale and then add the NaCN to the flask in the oil pan. The
oil pan should catch anything that falls (NaCN gives off HCN when exposed to
H2O and CO2). I found, also, If you do everything in front of a window fan
you can keep fumes down to a minimum. After the apparatus is set up, a
length of rubber tubing can be connected to it using an adapter or a one hole
rubber stopper and glass tubing(ie. top of condenser in a reflux system) and
the rubber tubing can be led through the window to the outside. The
speed of some window fans can be controlled (ie. variac or motor speed
control) which allows you to slow them down to keep the noise down (do this after
the reflux or distillation apparatus is set up).
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Mastermind
(Hive Bee)
07-22-00 14:49
No 31829
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Re:
P2P
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Here's a picture of the P2P tube furnace. The reason its warped is
because it was heated to 800 degrees C a couple times when making ketene from
acetone. It tended to soften at that temperature. Broken porcelain
saucers were used as the catalyst when making ketene. It was heated to
about 450 degrees for the P2P and about 550 degrees to dry or regenerate the
catalyst (with air blown through it). No softening was noticed at 550
degrees.
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LaBTop
(Moderator)
07-26-00 05:21
No 33319
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Re:
P2P
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Mastermind, I'm gonna include this in the "Detailed Methods for
Non-Chemists" thread, first in the thread in progress in the Methods
forum, so some more chem oriented people can interact, then when ready, in
the above final one.
It happens to be, that some friends of mine and me are also highly interested
in this method, and were allways baffled by the lack of interest here for the
method. It has been discussed earlier, as you may know, but starved as usual
a soft death.
This easiest synth of P2P, combined with my One Pot d,l-Meth synth, will open
the floodgates for all who want to make their own personal stash of
methamphetamine, instead of beeing surrendered to the faulthy tricks of
street vendors.
I will do my best to make a readable total write-up, and you can PM me for
further discussion, we have quite a lot of material on this, just as you.
The main cullprit for many seems to be the necessity of NaCN, which in fact
with the proper safety-measures forms not such a big thread at all.
Have all drawings etc., but that foto says much more.
As said before, I really would appreciate a safe, longstanding website
for dumping foto's, drawings and tons of text, this is the last time I ask
for it, there must be hundreds of you out there with the proper skills to
setup a website which won't be banned for such a purpose, just to dump stuff
so we can link in Markup to that website.
I really don't have the time to develop into a computerexpert besides my
other activities, I only pick up what I think I need for that.
It's the last time I ask, if no offers, you all will have to miss my, and
others, extensive library. LT/
WISDOMwillWIN
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Mastermind
(Hive Bee)
07-27-00 17:37
No 34004
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Re:
P2P
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I'd be interested in seeing what you have LaBTop. As for the need for a
web site for photos and drawings, why don't you set up an account at
www.geocities.com and put your images there? I set up an account and it
has my hushmail email address as about the only link to me (besides my ip
address). If you have a dynamic ip address it shouldn't stay the same,
anyway. Another thing that you might try if you want to eliminate all
traces (hopefully) is try a proxy to geocities.
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LaBTop
(Moderator)
07-28-00 04:10
No 34168
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Re:
P2P
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I give a shit about traces, that's not my concern, all you mention and much
more is used.
It's the extensive lot of work to download all that to a website of choice,
and then some moron admin will wipe it away because some bored housewife
complaints about the offensive and criminal content of it.
Look what happened to many known names' websites, suddenly they were wiped.
I'm not going to do weeks and weeks of work to get wiped because some
pathetic little moron passes by.
You would be surprised by the amount of visitors we have here who have only
one goal in life, to inflict as much damage as they can to this site and its
associate sites.
There are at the most about 200 people here who really know what they are
talking about, the rest is in the learning phase and would probably only dump
a lot of confusing bullshit on such a website.
I'm thinking about a system like McAfee Fortress password encrypted
self-executing files, a blind alley index page, and a unique alphanumeric
login page. All files will be password protected by the blowfish algorithm.
If we need one file or jpeg or video to link to, we put that on another
alphanumeric page, and provide the password here. So that moron can only
damage one page a time, and when it happens, we can track him/her down and do
some funny damage back. Never threat, just do. LT/
PS: it looks as if the bulk of you out there only is interested in taking,
not giving.
WISDOMwillWIN
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LaBTop
(Moderator)
07-28-00 13:46
No 34291
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P2P
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Not meaning Mastermind, ofcourse. LT/
WISDOMwillWIN
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placebo
(Hive Addict)
07-28-00 16:11
No 34317
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Re:
P2P
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I have been dieing to post some pics, just haven't got round to it yet, and I
don't think it would be a problem to have pics at Geocities you just don't
upload them to a page you have them sitting in your behind the lines files,
that nobody sees, you know where you put the pics you are linking to for your
webpages. Nobody can get in there except you and admin I suppose, but
definately no kids! I have had seedy pics at my website for 3 months and no
probs yet!
One
horny Bee!
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PolytheneSam
(Hive Bee)
02-01-01 19:09
No 170666
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Re:
P2P
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P2P process coming up for you, LeVogue.
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terbium
(Hive Bee)
02-01-01 23:51
No 170689
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Re:
P2P
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Yes, this would seem to be a good method that avoids the need for acetic
anhydride - glacial acetic acid is used instead. And the phenylacetic acid
can be made by oxidation of phenethyl alcohol. Phenethyl alcohol is what
gives roses their characteristic smell and should be available from fragrance
suppliers.
This may become a more popular method now that the authorities are making it
difficult to obtain rP. Constructing and operating the tube furnace can't be
any more of a hassle than obtaining rP from matchbooks.
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