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dickdastardly
(Stranger)
12-05-01 12:14
No 244534
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IS
THIS THE BEST OTC P2P Route
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Toluene and dry Calcium Hypochlorite (bleaching powder) are heated together
to 105°C in the abscence of other reagents. This avoids by-product formation.
If equal amtounts are used, volume-wise, there is a high conversion. If more
bleaching powder is used, the conversion is more robust, but contaminants
such as benzal chloride and benzotrichloride are formed [...]
10 pct. of a solution of 1250 g benzyl chloride [1] in 2500 ml of
sodium-distilled diethyl ether is added to 240 g magnesium turnings under
1000 ml ether, and a small iodine crystal is added. after start of the
grignard reaction the rest of the benzyl chlorideiis added with stirring to
maintain gentle boiling (if the reaction becomes too vigorous, useless
1,2-diphenylethane is formed) and the mixture is heated and stirred until
most magnesium is dissolved. The grignard reagent solution is poured on 1 kg
water-free, crushed dry ice (solid CO2) and stirred for 2 hrs. 2000 ml warm
ether is added and the mixture is heated in a water-bath until the internal
temperaturerreaches 25°C. 2000 ml hydrochloric acid 32 pct. is added, and the
heterogenous mixture stirred until any inorganic precipate is dissolved.
after filtering, the organic layer is separated, washed with cold water, and
dried over 200 g anhydr. sodium sulfate. the ether is distilled off, and the
rest is recrystallized from water, to yield 75 pct - about 1000 g -
phenylacetic acid.
Place 1000g phenylacetic acid and 3000g anhydrous (or trihydrate) lead
acetate in a distillation apparatus and heat. First an amount of water will
distill, and next phenyl-2-propanone in this destructive distillation, which
requires liberal application of heat. The distillate will separate into two
layers. The organic layer is separated and redistilled to give pure
phenyl-2-propanone, bp 105°C/10 mmHg or 216°C at atmospherical pressure.
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formula54
(Hive Addict)
12-05-01 12:42
No 244550
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Re:
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twice in the wrong forum.
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timsong
(Hive Bee)
12-05-01 13:04
No 244558
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Re:
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You can't generalize this as the best way, it may be the best way for you but
not for others, differing with what chemicals are available to other people.
For example, someone might be sitting on a nice barrel of ethylbenzene !
The methods that you have cut and pasted from other pages are well known, but
there are many other methods.
I don't know how much experience you have with organic reagents ?
You should always know the reagents you are making or using in detail,
because sometimes the reactions look much easier in text than they are in
practice, and a lot of the toxic and explosive potentials of these reactions
are left out !
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foxy2
(Distinctive Doe)
12-05-01 16:28
No 244663
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That sounds pretty darn good, if it works as stated.
What is the final yeild of P2P from 1000g of PAA?
I think the lead salts can bee recycled, thus saving the environment.
Do Your
Part To Win The War
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PrimoPyro
(Hive Addict)
12-05-01 16:45
No 244672
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Re:
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Holy Shit! Thats amazing!
I was thinking almost the exact same thing yesterday! Im serious. I
was reading Rhodiums website for an hour or so, having a hypothetical need
for P2P for the first time ever, and decided upon the same route from toluene
with one minor modification:
Instead of messing with the grignard processes, which can be difficult for
non-proffessional chemists, and costly as well, I decided upon:
toluene + Ca(OCl)2 --> PhMeCl + Ca(OH)2
PhMeCl + KCN --> PhMeCN + KCl
PhMeCN + H2SO4 --> PhMeCOOH
Ca(OH)2 + 2MeCOOH --> Ca(OOCMe)2
PhMeCOOH + Ca(OOCMe)2 --> P2P
foxy, the same document on Rhodium's page states that calcium or barium
acetate can be used as a substitute for lead acetate. This solves the little
environment issue quite nicely.
http://www.rhodium.ws/chemistry/phenylacetone.html#phenylacetic
and scroll down to the lead acetate method.
Ref cited: A. I. Vogel, Practical Organic Chemistry, 5th Ed. p612-613.
PrimoPyro
Vivent Longtemps la Ruche! STRIKE For President!
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timsong
(Hive Bee)
12-05-01 17:13
No 244686
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Re:
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As for a process that would be best for the kitchen chemist, I would lean
towards the methods primopyro uses.
But I must point out the extra needs presented to the basic kitchen chemist
for the reations:
Vacuum apparatus will be need to dry the calcium hypochlorite, and for
distilling the benzyl cyanide.
Dryice would also needed for the grignard stage
If you went for the standard way of producing benzyl chloride from toluene by
bubbling chlorine gas into it on relux (with UV light)and weighing the mix to
determine the stop of chlorination. This would avoid vacuum drying
procedures. But you would still need vacuum apparatus for the cyanide stage.
So some nice DIY vacuum setup would put the iceing on the cake for kitchen
chemist (we all await the final diagrams rhodium+bees are collating).
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foxy2
(Distinctive Doe)
12-05-01 17:31
No 244690
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Re:
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"As for a process that would be best for the kitchen chemist, I would
lean towards the methods primopyro uses."
Cyanide is not good for a kitchen chemist
Do Your
Part To Win The War
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PrimoPyro
(Hive Addict)
12-05-01 17:37
No 244695
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Re:
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Either is anything else they work with. Cyanide is a word. Acetonitrile vs. methyl
cyanide, oooh scary. Same thing.
If you do it right, you will be fine. H2SO4 is bad for you, the fumes...
Lye burns.
HCl corrodes everything in sight (gaseous)
PhMeCOOH stinks to the high heavens.
HgCl2 is a deadly poison, 2g will kill.
MeOH is poisonous.
Everything we work with is poisonous. So is ether for the grignard.
PrimoPyro
Vivent Longtemps la Ruche! STRIKE For President!
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timsong
(Hive Bee)
12-05-01 17:42
No 244701
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Re:
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Cyanide is not good for anyone, but in the interests of being easily made
with household apparatus, cyanides seem a simpler route than the grignard
(everything needs to be anhydrous) procedure. Magnesium can be quite
expensive buying privately.
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foxy2
(Distinctive Doe)
12-05-01 21:14
No 244802
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Re:
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I never said I was scared of cyanide. But it is not that easy to make,
buying it could raise terrorism concerns, and if your are a stupid newbee
doing this in your kitchen you could very easily end up dead.
Pyro
Stop being a dumbass. Take some HCl and dump it in that KCN and take a
big wiff, then tell me cyanide is only a word. I know its not that big
of a deal if you take precautions, but I don't really feel that useing
cyanide in a kitchen is all that smart. I would want a hood, call me a
wimp.
You are correct, nitriles are NOT a big deal, I use acetonitrile almost
everyday and I take no precautions whatsoever. But nitriles are not
anything like cyanide salts except in name, so your analogy was stupid.
timsong
If apparatus is a problem then you are not trying hard enough. Getting
hardware is relatively easy, while the chemicals are what is more difficult
and controlled. I think you might turn heads when buying kilograms of
cyanide.(TERRORISM)
Do Your
Part To Win The War
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dickdastardly
(Newbee)
12-05-01 22:18
No 244841
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Re:
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Your probably right. I was more or less just putting 2gether a general idea
on how to To go OTC all the way without having to fuck with any watched
chemical. Were I live Meth use has grown to epedemic proportions and
everything that is even closely related to making meth is taboo. Just the
other day I walked into a convienience store and asked if they had vicks
inhalers and the lady behind the counter says to me "They don't make
them anymore because people were using them to make meth". How crazy is
that shit. You'd think I asked the brodd for Red P and Iodine crystals or
something.
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Shard
(Stranger)
12-06-01 00:33
No 244868
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Re:
IS THIS THE BEST OTC P2P Route
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Hell I'll admit it, cyanide scares me, as does barium, or am I just being
ignorant on that one?
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timsong
(Hive Bee)
12-06-01 00:43
No 244873
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Re:
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Reply to Foxy2:
The synth for cyanide is very simple using an OTC photographic chemical.
(Think laterally)
I don't have a problem with glassware/labware myself, I was thinking of
someone on a minimal budget.
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foxy2
(Distinctive Doe)
12-06-01 02:18
No 244900
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Re:
IS THIS THE BEST OTC P2P Route
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oh yea, i forgot about that synth.
Do Your
Part To Win The War
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Buster_Hymen
(Hive Bee)
12-06-01 13:20
No 245044
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Re:
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potassium ferrocyanide?
(used for cyanotype print processing)
\\|//
ô¿ô -- Semper ubi sub ubi!
\O/
'''
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Bozakium
(Hive Addict)
12-06-01 16:23
No 245121
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Re:
IS THIS THE BEST OTC P2P Route
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As TimeSong said, where the heck did Dick paste this together from? No
references, details or safety info.
It is presented in "cookbook format" like it is a synth that has
been done or could bee done as stated, given that weights, partial procedures
and product analysis is given. BUt it needs more info on the procedure, and
details about the Grignard step since it is one of the touchier reactions we
often come by. Other info like Glassware must be dried in an electric oven
prior to use, etc. Et2O can go boom in the still, would be nice for the
cookbookers, too.
Maybe he assumes we're Griggy experts, but a serious chemist
would always include a list of references to his procedure for background and
procedure details, and info on substitutiona and variants. Where's the refs?
He goes on to tip us off that something's wrong in Denmark when he
mentions destructive distillation in the last paragraph. Destructive
distillation is done in the absence of air, and there's no mention of an
inert atmosphere. Plus, were not destroying anything, its supposed to be a
reduction from -COOH to ketone.
I agree with timesong and ppyro. Cyanoide is a functional
group not to be confused with HCN the typical poison. Cyanide
containing compounds are not mega-dangers unless you eat them or mix
them with the wrong reagents and free some HCN.
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Rhodium
(Chief Bee)
12-06-01 22:32
No 245209
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Re:
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Dick has just copied some text from http://www.rhodium.ws/chemistry/phenylacetone.html
and the precursor links therein, the references are on my page.
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dickdastardly
(Newbee)
12-07-01 01:22
No 245239
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Re:
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Whoa hold on there . I was only asking a question in regards to the
feasability of the procedure. I totally agree with you Bozakium more research
should be done before any kind of synthesis of this type should be done. What
I was merely doing was putting together a procedure and looking for some
feedback on whether or not it is indeed workable
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Aurelius
(Hive Bee)
12-07-01 10:04
No 245343
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if it has made it onto Rhodium's page you can be 99%+ certain that the
procedure will work if performed properly. however, that all depends on
your own abilities.
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timsong
(Hive Bee)
12-07-01 14:27
No 245403
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Please don't take me the wrong way Dickdastarly, your post is highlighting a
path that newbees would find interesting, you have obvious been doing some
research. I only wanted newbees to realize that though it looks easy, a lot
more needs to been known about each stage before an inexperienced wannabe
starts trying it as if it were a cookery recipe.
Buster_Hymen, you mentioned Potassium Ferrocyanide !
yes correct.
Potassium Ferricyanide is a more widely used photographic chemical, that can
easily be converted to the 'ferro' with hydrogen peroxide solution. Potassium
Ferricyanide is a very commonly used photographic chemical and is normaly
called Farmers Reducer.
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PrimoPyro
(Hive Addict)
12-08-01 19:38
No 245762
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Re:
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foxy: perhaps I came off too sarcastic? Well, I agree with you on most
points, including my analogy.
I still think however, that cyanides are not a problem as long as acids arent
present. In this case, have a tube leading from the reaction flask into a
solution of NaOH to trap any possible evolved HCN.
PrimoPyro
Vivent Longtemps la Ruche! STRIKE For President!
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foxy2
(Distinctive Doe)
12-08-01 19:54
No 245765
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I completely understand what you meant as I feel the same way usually.
Fuck the safety just let me do it how I want to do it and leave me alone 
But I shy away from telling other people to fuck safety because I would feel
bad if they ended up dead. But me on the other hand, if I end up dead
then its my own stupid fault. 
Do Your
Part To Win The War
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epistemologicide
(Hive Bee)
12-09-01 04:41
No 245818
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Re:
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oi beez, alot of us are willing to learn and help, alot of beez would relish
worloks style(synths step by step) of basic understandings,
just some thing to consider,
ill always post in that style, it keeps things simple.
hatred
of ontological wastes, and the marathon!!!!
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lugh
(Hive Bee)
12-09-01 08:34
No 245848
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Re:
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Anyone that experiments with cyanides must bee very careful, acids are the
greatest danger, but many have died by accidental oral ingestion 
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timsong
(Hive Bee)
12-09-01 09:36
No 245861
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Re:
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By the way, if bees are gonna be going down the cyanide route, always have
some poppers (amyl/butyl nitrite) close, to have a good huff on if there is
any suspicion of cyanide contamination or poisoning.
(by the way, this won't save your life if you have received a high dose)
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timsong
(Hive Bee)
12-09-01 10:22
No 245868
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Re:
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As for the chlorination of toluene to give benzyl chloride. After looking at
the boiling points of toluene,benzyl chloride and benzal chloride is would
appear to be a good idear to always have slightly less of the calcium
hypochlorite (or chlorine, depending on which synth you are using) that is
needed, as the boiling points of toluene and benzyl chloride are 68c apart.
Much easier to fractionate than benzyl chloride and benzal chloride with a
difference 27c.
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PVnRT_NC8
(FMAN)
12-09-01 11:48
No 245890
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Yes but this would provide simply cross extrapolation datum
there has to be simple reliable and not so much in a hurry ways [like
vinagear makes pickles?]such explosive situation and the stench I used to
pour this shit out down the drain and sorta giggle as I did so, it drove
people plain fucking raving mad, anyone who thinks there is a shortage of
dope is mistakenly wrong........the climate is hostile to educational types
.....fundementalatists, not terrorist
Terrorist tactics and ohum my favorite Einstenium quote might be found on
Rhod's yet by some lurker out there???
More laws more crime more lawbreakers um its relitivity?
I like my salt plain with moonshine thanks anyways
Get rid of everthing but the still all other flamable gasseous threats shall
be reconsidered at a later time of course respectively I LIKE BATTERY ACID
FLAVORS
Amethystium
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timsong
(Hive Bee)
12-09-01 12:08
No 245899
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PVnRT_NC8,
are you trying to say that meth bees should just give up and let the big boys
carry on pumping out the stuff ?
If it wasn't for apprenticies, there would not be anyone to replace the
busted and retired chemists.
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lugh
(Hive Bee)
12-09-01 12:08
No 245901
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Re:
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For more information about benzyl chloride using calcium hypochlorite and
toluene, including a procedure for separating the toluene/benzyl chloride
azeotrope, see Post No 36700
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