Author Topic: nano and rp/i suck try this instead  (Read 8050 times)

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quantum

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nano and rp/i suck try this instead
« on: February 22, 2004, 11:28:00 PM »
well ive tried heaps of rp/i synths and ye they work but
the process is a pain in the arse and all of the tabs
and chems are now watched so why not go for the imine gringnard.

toluene + calcium hypochlorite (paint thiner and pool bleach) --->  benzyl chloride

benzyl chloride + magnesium (fire lighters at desposal store) -----> benzyl magnesium chloride

ethanol + potassium di chromate + sulfuric acid ( metho + photo developing chem + battery acid) ---> acetaldehyde
ethanol + sulfuric acid ---> ether
any of the many methylamine synths I think I will try
to do an Al/Hg on nitro in ether then filter Al(OH)2 sludge
keeping ether/methylamine solution.

methylamine + acetaldehyde ---> acetaldehyde methyl imine

acetaldehyde methyl imine + benzyl magnesium chloride --->
racmic meth major dex minor lev

why waist time making rp/i when in a one litre flask you
can do this and end up with over 100 grams per shot.
high yeilds from what ive read and I have checked all of
these synths out in my orgranic synthises and they all
seem to check out nice.
maby its time to leave these stupid fucking pills alone
and do some real chem.


lugh

  • Guest
Not as easy as it sounds
« Reply #1 on: February 22, 2004, 11:48:00 PM »
You're right in stating it all makes sense, but none have reported success but L_L, and many others have tried  ::)  One flaw in your proposed synthesis is that magnesium fire starters aren't pure enough for a grignard, you would have to form the chloride, purify it and use the OS method to prepare the Grignard reagent  ;)


ChemoSabe

  • Guest
Get Busy with it Then!
« Reply #2 on: February 22, 2004, 11:49:00 PM »

quantum

  • Guest
fucking magnesium
« Reply #3 on: February 22, 2004, 11:54:00 PM »
so I have to get it from a chem supply place damb.
any way that I can tell if the fire magnesium is good or not
ive seen a few different types around.
maby if I used lithium instead and did the gringrnard in
dry ice instead then I can make the lithium pure as from
lithium carbonate


jemma_jamerson

  • Guest
or may i suggest
« Reply #4 on: February 23, 2004, 04:28:00 AM »
ethanol + potassium di chromate + sulfuric acid ( metho + photo developing chem + battery acid) ---> acetaldehyde

+toluene ---> benzaldehyde (ha just found a funny link

http://www.faizkaskar.8k.com/proj.htm


on MANUFACTURE OF BENZALDEHYDE BY LIQUID PHASE CHLORINATION OF TOLUENE..)

for the bio synth of l-pac..then catalytic hydrgenation---->meth


frosted

  • Guest
Magnesium.
« Reply #5 on: February 24, 2004, 10:03:00 PM »
If you have a way to get pure magnesium, is this synthesis possible?  Is the magnesium purity the only problem with this synthesis?  There is a factory close by that produces products made of magnesium, so swim could get some scraps from there and use that.  Unless there is something else wrong with this process as well.  Any insights?


RepVip

  • Guest
Ether
« Reply #6 on: February 24, 2004, 11:24:00 PM »
My two cents:
You should have a way easier time obtaining LG magnesium than making your own diethyl ether...
Also you would need some practical lab experience and the proper glassware (of course) to do most of the synths you suggest. Its not as easy as it sounds, however, I am in total agreement that this is a better way than the mbrp/I(tincture), at least for some.

Organikum

  • Guest
lugh ?
« Reply #7 on: February 25, 2004, 08:24:00 AM »

you would have to form the chloride, purify it and use the OS method to prepare the Grignard reagent




Assuming that "OS" stands for Osmium and the "chloride" refers to  magnesium, I did a search for this method using "grignard" and/or "MgCl" etc. but came up with nothing.
Can you point me to this please?

thanks
ORG




lugh

  • Guest
Organic Syntheses
« Reply #8 on: February 25, 2004, 12:10:00 PM »
OS is an abbreviation for Organic Syntheses, see

Post 448168 (missing)

(WizardX: "GRIGNARD AND RELATED REACTIONS", Stimulants)
 ;)


Organikum

  • Guest
Oh !
« Reply #9 on: February 25, 2004, 02:17:00 PM »
me stupid  ;D  :(

Actually my first guess was "Operating System" - must be related to my profession... :)

thanks
ORG (not synthetic)

EDIT
But following this links shows me ALL Grignard reactions at Org.Synth. what is nice but not new to me. Sadly it answers in no way the question on WHICH Org.Synth. procedure was talked about. The one link provided by WizardX which MIGHT have been it "preparation..." leads to nowhere....
Sad but true.

"Da steh ich nun ich armer Thor and bin so klug als wie zuvor..."
Goethe, Faust.  ;D


skanic

  • Guest
benzyl magnesium chloride synthesis
« Reply #10 on: February 25, 2004, 05:32:00 PM »
hello,
what is the yield of the benzyl magnesium chloride synthesis, if BzCl and Mg are pure ?
can we use an other solvent than diethyl ether ?

quantum

  • Guest
hehe
« Reply #11 on: February 26, 2004, 01:17:00 AM »
as usual give em a bone and they want ya leg :)
well as far as can it be done in other solvents the answer is yes and maby you would have benifeted more by reading
the gringnard links lugh produced becouse then you would
know why. this attitude that a lot of the hive has kills me
the only question we should be asking is why is that not
what science is about why use ether for a solvent.
come up with that answer and you will find that you can
use THF or even dibutylether.
I have heard rumours of being able to do the second part
of the gringnard in an aromatic solvent but the first
part to my belife is catylized by the oxygen in the ether.
so to answer correctly yes and no. but then if you were
interested in chemistry and not your nose and pocket
you would have known that.
yes this works yes lugh is right about the firestarters
and yes it is easier to buy somthing from a shop than
to synth ether. but if you cannot synth ether what the
fuck are you doing making drugs for human consumption.
this place is a freedom but dont ever forget it is also
a responsability.

now for another idea (not mine just puting it in everyones
face)

toluene + hypochlorite ----> benzylchloride
potassiumferricyanide + sulfuric acid ----> hydrogen cyanide
hydrogen cyanide + sodium hydroxide -----> sodium cyanide
benzylchloride + sodium cyanide -----> benzylcyanide
benzylcyanide + sulfuric acid ----> phenylacetic acid
acetone via pyrolysis -----> keten
keten + water ----> acetic acid
acetic acid + keten -----> acetic anhydride
phenylacetic acid + acetic anydride with a dash of sodium acetate ----> phenyl-2-propalacetone

potasium ferricyanide is used for photography and blue prints.

be warned hyrogen cyanide and keten are fucking deadly.
SO DONT TELL ME I FUCKING KNOW.


peace all and keep reading rp/i'ers your time is nearly up
and thank fuck for that


skanic

  • Guest
thanks
« Reply #12 on: February 26, 2004, 11:40:00 AM »
thank you quantum

stereoIsomer

  • Guest
yes- thanks quantum, and a note on the toluene
« Reply #13 on: February 26, 2004, 09:07:00 PM »
Thanks for teeing up this pathway, quantum. I was told (by someone who knows, 2+ years ago) that meth was being synthesized industrially in the Americas via Toluene as initial building block. So, it should be encouraging to know that it's being done successfully as a large scale process this way. Whatever i can find out further about details, I will certainly post.

The note on TOLUENE:::
On the left-coast, some large DO-IT-YO-self supply warehouses no longer carry TOLUENE. Whilst shopping in the PRO SHOP of one of these orange & black behemoths, I was told by the floor-hand that Toluene's role in drug synthesis was the reason it is no longer on shelves.
Fortunately the asian hardware store up the street sees no such conflict of interest- so at least it's not law out here. Nonetheless, this could be a trend and as always, be careful buying- it's possible to track (solvent) purchases over time to individuals, if for no other purpose than 1:1 marketing / data-mining........

peace!

frosted

  • Guest
So is this all theory?
« Reply #14 on: February 26, 2004, 10:17:00 PM »
So is this all theory?  Or can this actually be done? Has anyone tried it yet?


WizardX

  • Guest
Updated links
« Reply #15 on: March 03, 2004, 12:53:00 PM »
GRIGNARD AND RELATED REACTIONS

http://www.orgsyn.org/orgsyn/RxnTypes/section.asp?section=117



HIGHLY REACTIVE MAGNESIUM FOR THE PREPARATION OF GRIGNARD REAGENTS

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv6p0845



n-PROPYLBENZENE, C6H5CH2CH2CH3

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0471



Catalytic Dehydrogenation
C6H5CH2CH2CH3 ==[-H2]==>> C6H5CH=CHCH3

quantum

  • Guest
fucken legendary
« Reply #16 on: March 03, 2004, 11:25:00 PM »
nice on wizard so now onto making potassium :)
do you think that K will strip Mg of a sulfate ion
as well as the chloride?


quantum

  • Guest
nope just found the answer
« Reply #17 on: March 03, 2004, 11:39:00 PM »
no can do only halides intersting that you can use Na as
well


ahgreich

  • Guest
MEK + Benzaldehyde
« Reply #18 on: March 04, 2004, 07:21:00 AM »
Benzaldehyde + MEK acid catalyzed aldol
simplest route to P2P that sb had seen lately. nothing foul like ketene or benzylchloride.

quantum

  • Guest
yes I know of that one :)
« Reply #19 on: March 04, 2004, 08:06:00 AM »
but I am not so sure on the yeild of the beayer villiger oxidation. it all looks great untill you need some funky
oxidizing agent to get over 30% yeild yucky

just did the first step benzylchloride from toluene well
its running now everythings sweet used 200g of hypochorite
and an excess of toluene hoping not to get any di and tri
halides cooking it on a water bath and there is no risk of
explosion or fire.
I have kept the temp of the water at around 95 C so as not
to loose heaps of water (im not in the lab at the moment)
and there are lots of little bubbles all over the place inside the flask, very smooth indead :)
will let you know how I go and post yeild based on hypo
tomorrow boiling battery acid then NaCN :) from ferricyanide
if I dont post nice knowing ya all.


amalgum

  • Guest
Re: but I am not so sure on the yeild of the...
« Reply #20 on: March 04, 2004, 11:33:00 AM »


but I am not so sure on the yeild of the beayer villiger oxidation. it all looks great untill you need some funky
oxidizing agent to get over 30% yeild yucky




Yes, and if yeilds were over 30% this would be the ultimate method.

However, SWIM doesn't think 30% is all that bad either.  The procedures are much quicker, and much easier than those invovled with the classic toluene to chloride, to cyanide, to phenylacetic acid then p2p method (which SWIM has attempted recently with some success). 

SWIM is one who started with rp/I2.  So being able to spend half the money, and whip up hundreds of times of product as the equivalent of rp/I2 methods is like a dream in a dream.
SWIM had haphazard technique at the time SWIM attempted the classic p2p route, and yeilds were low then anyway and there were many steps and tedious distillations especially.

If you can get toluene cheaply and abundantly like SWIM, then that route is still very lucrative.  One day SWIM was bored (and tweaking) and calculated potential % of profit from the cost put in of all solvents/reagents (glassware on hand, not figured in) needed for 1/4th pound of end HCl product.  Also used average price potential of 1/4th pound in my area, and figured in things like personal usage, error correction etc (I was really jacked up).  It came to like 786% profit or something.  That was for the aldol/bayer villager route.


bio

  • Guest
if yields were over 30% this would be the ultimate
« Reply #21 on: March 05, 2004, 11:07:00 AM »
Second try got 39% and that is being improved. If you read the patents by recycling they got quant. Working on this and sulfuric as catalyst. Also the dilution factor has been halved and the MePhBuO yield is up 25%.

 Do some research. I think 60% yields are possible without a fancy solvent or catalyst. With those in the review Rhodium just posted quit high yields would be possible without recycling which only makes sense if you are doing one batch after another.

It is a lot of work but nothing compared to starting with what i've read in this thread. By the time you get to the last 2 or three steps you will be begging for mercy w/o real lab experience ::)  :)  especially when you end up with 50 grams for 6 weeks work.

amalgum

  • Guest
Shit, not even half of the work compared to...
« Reply #22 on: March 05, 2004, 07:32:00 PM »
Shit, not even half of the work compared to other methods SWIM has tried.  Yeah it would suck to do all that and come out with barely anything, but SWIM is in it more for the chemistry than anything else.  SWIM likes to tinker.  Also all procedures involved are really easy, all SWIM would have to obtain equipment wise is new vacuum pump (old one is peice 'o shit), everything else is on hand (SWIM spent big bucks on glassware).  Peice of cake!

Right now money is a limiting factor for SWIM, so when the available funds arise SWIM will be trying that route out for sure.

bio

  • Guest
likes to tinker.
« Reply #23 on: March 05, 2004, 09:08:00 PM »
So many routes from PhCHO which you can make from PhMe with MnO2/H2SO4 or in a  stainless steel furnace tube with air as oxidant and various catalysts. I used Cerium Molybdate for over 90% yield. Hell you could even use the same tube to make your P2P.

Get MnO2 or MnCO3 from a pottery supplier or lantern battery if you don't want to deal with chem suppliers. If you don't want to buy List One stuff EtNO2 can be made quite easily from EtOH & Nitric acid per US4431842. Nitric acid is real cheap and you don't need much and it's not as suspicious as many seem to think. In all these years having bought just about everything in the book (not List One) no supplier has ever asked me what is it for.

quantum

  • Guest
ill try both :)
« Reply #24 on: March 09, 2004, 03:38:00 AM »
yep made the chloride not very high in yeild though it
worked man that stuff is horrible.
I havent made the cyanide yet though I have made ketene
and AA from it. the ketene was very easy with no problems.
so far I have 150g of chloride ill keep on making it
for the next two weeks by the look of it and I will make
a heap of benzaldehyde as well to do the aldol.
I was very disapointed at how low the yeald was for
the chloride synth and this is with a 1000W HPS and a 33W
fluro. though I have done three synths of the choride now
and each one is getting better.
maby ill make some aldehyde tonight have to see if time
permits.
ive got about 500g of NaNO2 for food use and have heard
something from rhodium about using it with styrene to get
to P2NP not so sure what he means though (like nitrosite of
isosafrole or somthing).
dont worry 6 weeks work for 50 grams is not such a big prob
lets say I sell that for around $100 (not us) per gram
which is not to hard here thats over $800 per week.
im not realy wanting to get rich out of this just free of
aquiring drugs from others and able to help thouse I know.
is it possible to distill meth freebase with out a vacuum
and if not how much vacuum do you need before it deteriates
word of warning to thouse who follow the choride will make
you angry give you headaches problems with your eyes and
nose and it feels like DCM when it gets on your skin (though
the pain lasts a lot longer. I would say this is due to
the aromatic in the chem)
is this shit going to make me sterile the thought has been
in my mind for a few weeks now and after the chloride
I have my suspicians.
thanx for the posts


Organikum

  • Guest
I guess that methamphetamine freebase can be...
« Reply #25 on: March 09, 2004, 01:53:00 PM »
I guess that methamphetamine freebase can be distilled at STP without breaking down, but I would advise steamdistillation as this works like a charm. You dont even need an external steamsource - just put enough water in the flask - dont make it to full though - and here you go, nothing easier than this and very good results. Distilling directly into diluted HCl (10%) gives the salt immediately this should be recrystallized lateron.
DCM hurting on the skin is new to me, but BzCl is the shit, even worse than chloroacetone IMHO - gloves and better ventilation/improvised fumehood are advised.

good luck furtheron!


amalgum

  • Guest
I don't think I would attempt STP distillation
« Reply #26 on: March 10, 2004, 09:26:00 PM »
I don't think I would attempt STP distillation of the freebase at all, unless it was steam distillation of course.  However, thinking of most reductive amination methods from the ketone, SWIM would steam distill at the least, and highly reccomends using vacuum distillation instead.
If your not using vacuum how do you plan on purifying that P2P?  Steam distillation of the P2P (esp. from BzCl) probably will fuck up red. admin. giving low yeilds or maybe worse (due to impurities).  Vac. distill.  Maybe you can get by with a steam distillation and then purification with bisulfite.  SWIM suggests running a TLC plate on finished ketone to be sure (trust me those kodak pre-coated plates are worth it).



DCM hurting on the skin is new to me, but BzCl is the shit, even worse than chloroacetone IMHO - gloves and better ventilation/improvised fumehood are advised.




Heh, SWIM made benzyl bromide one time thinking it would be easier.  First of all, fucking with home made bromine is a BEOTCH!  Second, just taking apart the apparatus and washing it brought tears to SWIMs eyes, and burned those membranes like snorting a red hot coal!


amalgum

  • Guest
Oh yeah almost forgot......
« Reply #27 on: March 10, 2004, 09:35:00 PM »
Oh yeah almost forgot......
Right now the majority of SWIMS equipment/chemicals is a couple hundred miles away, trying to arrange a trip to go retrieve them soon (within a week or two), then SWIM will be tinkering with the above methods once again!
Also, SWIM was doing some research on hydratropic aldehyde the other day.  This might be another option SWIM wants to tinker with if a good preferrably OTC source of cumene can be found.  SWIM was thinking of using some of his dichromate salts, NaCl and H2SO4 to get chromyl chloride.  Then SWIM will use that to oxidise the cumene to get hydratropic aldehyde. SWIM is still looking for more info on cumene oxidations (of all types, mainly details on the chromyl chloride route), so anyone out there with any info on this, SWIM will be glad to see it.
This can be a great route potentially.  Just three major steps to meth from cumene.  Oxidation to HTA, then H2SO4 rearrangement to phenylacetone, followed by red. admin.

b159510

  • Guest
Meth heads do real chem?
« Reply #28 on: March 11, 2004, 08:37:00 AM »
This is your suggestion for replacing the rP/I rxn? Grignard, completely dry conditions, dichromates, etc? Forgive me for saying so, but it seems like you don't understand why the rP/I rxn became popular to begin with.

Even for those meth freaks who have to scrape matchbooks and extract from tincture, I imagine your method posted here would not be considered an improvement to them. I doubt they could even pull it off, and just might need to have some nice iodine crystals anyway to kick-off their less than shiny Mg from a lighter and their not so dry BzCl and homemade Et2O. (If they didn't scratch out their eyes from the BzCl before they even got to the Grignard.)

True though, as you mentioned, if you can't get the pseudo you will need alternatives. If you have the skills etc. to go this way then you can probably do the hydrogenations, which are way cooler (IMHO) if you want to 'do some real chem'.

Have fun and try not to kill yourself.


amalgum

  • Guest
I never said that the above methods will ...
« Reply #29 on: March 11, 2004, 01:41:00 PM »
I never said that the above methods will replace rp/i2.  I was merely thinking aloud sorta.



This is your suggestion for replacing the rP/I rxn? Grignard, completely dry conditions




Nope, SWIM tries to stear clear of Grignards.



dichromates, etc? Forgive me for saying so, but it seems like you don't understand why the rP/I rxn became popular to begin with.




As for the dichromates, hell yeah SWIM is going to tinker with that.  Fuck the rp/i2, and toying with gakked pills.  Don't get SWIM wrong, SWIM still imploys the rp/i2 himself, esp. cause the majority of his equipment isn't with him right now.  SWIM already has ~80% of the required chems for many different phenylacetone routes (plus for routes to many other exciting things SWIM wants to fuck with in the future, hrmmm theres hydroquinone for 2C-B and DOB, got a couple of kilos of eugenol laying around for future ether cleavage and methyleneation for those beloved methylenedioxy derivatives, need I go on?) just laying around. 
Also I am not a dumbass, the rp/i2 is put forth in such a way so the non-chemist crowd could make speed, which is why it's so popular.  Most people don't wanna sit and teach themselves advanced concepts and theory's of organic chemistry.  SWIM himself eats and sleeps and breathes O Chem., and plans to make it his life long career (legally that is, R&D baby!).  Since SWIM is fortunate enough to know how to pretty much search around and find things on his own (can't remember the last time SWIM asked a real question on any of the boards he visits), and has accumulated thousands of greenbacks worth of glassware (never send me a catalogue, SWIM'll go broke), not to mention the required technique and igenuity, so you are damn right the idea of much much larger scale production for a fraction of the cost of rp/i2 methods. Trust me, SWIM has done the math and even figures in for fuck-ups/errors etc.



Even for those meth freaks who have to scrape matchbooks and extract from tincture, I imagine your method posted here would not be considered an improvement to them. I doubt they could even pull it off, and just might need to have some nice iodine crystals anyway to kick-off their less than shiny Mg from a lighter and their not so dry BzCl and homemade Et2O. (If they didn't scratch out their eyes from the BzCl before they even got to the Grignard.)




SWIMS speculations were definitly not intended for newbee's or non-chemists at all, but only for those skilled properly in the art.  SWIM STRONGLY suggests these methods for those only with the proper experience/equipment/knowledge. Otherwise your right, a lot of non-chemist people will end up botching and or hurting/killing themselves or others. Esp. if attemtping less traveled routes to p2p and they don't know shit about things like quantitative/qualitative analysis or even something simple like proper fractionation technique.  Anyways, let me end this tangent and say my last rebuttal.



True though, as you mentioned, if you can't get the pseudo you will need alternatives. If you have the skills etc. to go this way then you can probably do the hydrogenations, which are way cooler (IMHO) if you want to 'do some real chem'.

Have fun and try not to kill yourself.




Damn right!  Fuck pseudo, SWIM enjoys the buzz of good ole prope dope anyway.  Your also right about hydrogenations being cooler, esp. the internal type ran on a certain imine.

As for killing himself, SWIM has plenty of experience, reads Vogel and others like it was a holy bible and such.  Plus SWIM has used other routes to acquire p2p before, and has tinkered with a couple of red. admins.  SWIM has had the joys of the associated paranoia when working with those lachyromators like benzyl halides, and also things like cyanides (better beleive SWIM totally re-vamped ventilation issues for that last one, as well as stocking up on amyl nitrate poppers for antidote purposes, just in case).

SWIM is carefull, does plenty of the right research, doesn't rush anything and has known limits of things SWIM will not do with current lab setup due to health/safety risks etc.  SWIM takes great pride in quality of synthesized products.  If there is anything worth doing, it's worth doing RIGHT!


quantum

  • Guest
just passing through
« Reply #30 on: March 23, 2004, 04:07:00 AM »

ADDkid

  • Guest
Dude you are giving me a headache, with your...
« Reply #31 on: March 24, 2004, 04:09:00 AM »