Author Topic: New Route to Meth  (Read 7775 times)

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dwarfer

  • Guest
New Route to Meth
« on: February 04, 2004, 11:11:00 PM »
This is more a chemistry matter than stimulant  IMHO..

:P
New route


16.5 grams (0.1 mole) of pseudo-ephedrine
is dissolved in 10 ML benzene
and placed into a  SS Pipe of volume 250 ML 
with threaded end caps
fitted with a pressure gauge and needle valve,
to which is added 2ML (approx 0.1 mole) H2O.

8.2 grams (.2 mole) CaH2
is placed in a ceramic "boat"
floating on the combined liquids.

The threaded SS end cap with the pressure gauge
and needle valve is screwed on tight
with Teflon sealing provisions.

The sealed unit is upset,
allowing the CaH2 to contact the H2O.

The reactions are:

CaH2+H2O >CaO + 4(H)^
CaH2+(OH)>CaO + 3(H)^

0.7 mole volumes gaseous H2 = (22.4 liters) x (.7)= 15.65 liters (stp)

By Boyle's law, P1V1=P2V2

[15.5 liters produced gas (rounded) / 0.25 liter volume] x (14.5 PSI  ) = 900 PSI


The second reaction reducing the alcohol
may not be favored in the basic conditions,
in which case the pressure will be slightly more
than 500 PSI, in which case
you start over with a 125 ML SS pipe,
(getting the pressure back to around 900 PSI)
and shake it on your vibrator,
measuring the pressure drop over time.  

The experiment might also be conducted
with the pseudo.HCl salt dissolved in water,
but it would take a molar excess of water
to dissolve the salt,
in which case you would have Ca(OH)2 basic water with FB.

A third reaction in this case would be
CaH2 + 2(HCl)> CaCl2 +2(H2)^

The needle valve would be used to vent over pressure mistakes,
and to drop the pressure after the process is done.

Works like a charm every time: in my mind.?????

::)


Please disabuse me gently of my pretentions,
as I am only an humble cogitator of dreams,
drifting in comfortable illusions....



SPISSHAK

  • Guest
hmmm???
« Reply #1 on: February 05, 2004, 12:16:00 AM »
sounds like a pipe dream pun intended

josef_k

  • Guest
Assuming everything else worked, I think you...
« Reply #2 on: February 05, 2004, 12:57:00 AM »
Assuming everything else worked, I think you would need a hydrogenation catalyst like palladium on carbon.

dwarfer

  • Guest
Calcium Hydride Properties: Orthorhombic ...
« Reply #3 on: February 05, 2004, 01:49:00 AM »
Calcium Hydride

Properties:  Orthorhombic crystals or powder; the commercial product is gray.  d 1.7.  mp 1.86°.  Decomposes with water, lower alcohols and carboxylic acids to form hydrogen; moderately powerful condensing agent with ketones and acid esters; more powerful reducing agent toward metal oxides than lithium or sodium hydrides.
Melting point:  mp 1.86°
Density:  d 1.7
Use:  To prepare rare metals by reduction of their oxides; as a drying agent for liquids and gases; to generate hydrogen:  1 g of calcium hydride in water liberates 1 liter of hydrogen at STP; in organic syntheses.

=======================

Well, I was hoping maybe...??


wareami

  • Guest
Tenacity....
« Reply #4 on: February 05, 2004, 02:00:00 AM »
Ya really gotta admire the Big D's tenacity as well as his "Dickaround of the Year" diploma! ;D
Simply amazing!!! :)



methymouse

  • Guest
Uhhh
« Reply #5 on: February 05, 2004, 02:06:00 AM »
"Decomposes with water, lower alcohols and carboxylic acids"

Umm, like MeOH and EtOH?  If I understand correctly, this means primary alcohols--not secondary alcohols (like pseudoephedrine).


dwarfer

  • Guest
lower alcohols
« Reply #6 on: February 05, 2004, 03:23:00 AM »
I thought a secondary benzyllic alcohol would qualify
as a lower alkie.

I  woulda thought about some surfactants: maybe some glycerine type alkies as not subject to be considered as a lower alcohol.

 Isopropyl alcohol; : do you think CaH2 would snatch the oxygen? It's a secondary alkie, is it not?


Seems to me that it maybe might on a good day..

ah never mind :(

thanks for the vibe, Ware:
I ran it up the flagpole,anywayze.



Rhodium

  • Guest
Calcium hydride + any alcohol -> calcium...
« Reply #7 on: February 05, 2004, 04:30:00 AM »
Calcium hydride + any alcohol -> calcium alkoxide + hydrogen gas


It won't reduce anything though.


WizardX

  • Guest
CaH2
« Reply #8 on: February 05, 2004, 05:22:00 AM »
CaH2 + 2H2O ==> Ca(OH)2 + 2H2

WizardX

  • Guest
Don't give up!
« Reply #9 on: February 05, 2004, 10:35:00 AM »
dwarfer: Don't give up! Work along the line as such. CaH2 + haloephedrine in a super dry ether.

CaH2 + 2 C6H5-CH(-I)-CH(-NHCH3)-CH3 ==[super dry ether]==> 2 C6H5-CH2-CH(-NHCH3)-CH3 + CaI2

The CaH2 will not dissolve in the super dry ether so vigorous stirring (magnetic stirrer) is required to keep it finely divided.

You can test the progress of the reaction by adding the CaI2 precipitate to some water. CaH2 reacts quite rapidly (almost violently) with water. CaI2 only dissolves.

methymouse

  • Guest
Maybe
« Reply #10 on: February 05, 2004, 03:54:00 PM »
That might work, though it's a bit unclear to me how you iodinate without HI.  On the other hand, HBr is readily available, and one can supposedly synthesize chloroephedrine with ZnCl2 (glass flux) and HCl.  UTFSE for "Lucas Reagent."  Best of luck.


dwarfer

  • Guest
haloephedrine
« Reply #11 on: February 05, 2004, 07:18:00 PM »
wiz: can it be chloro-ephedrine?

rhode:  so you get "ephedrine alkoxide".  big whoop.  I can see how you have to swap the (OH)  for a nicer leaving group. :( [sad]

wiz:  I guess the CaH2 would MAKE it a super dry ether: would having some water to generate the H2 be of value (with CaO made because of the molar excess of CaH2 {Rhode said the reaction proceeds thru CaO to Ca(OH)2 with a surplus of water only.

Would there be any advantage to pressure?

 
Seems to me there is still some hope, then.

the reaction should be quantitative with the halo
intermediary with no apparent side over-reaction
problems.  the limitation would be the making of the
chloro-ephedrine,(which I think is made more efficient
in the microwave).

Seems like this might be a ton easier than the electro route,
with similar qualities..  ?? ::)


dwarfer

  • Guest
lucas reagent refs
« Reply #12 on: February 05, 2004, 07:37:00 PM »
[

http://www.angelfire.com/scifi/WizardX/index.html

]
thanks Wiz
[

http://science.csustan.edu/stkrm/Recipes/Recipes-Lucas.htm

]
[

http://nlfaculty.dcccd.edu/logan/slides/chapter10/sld026.htm

]

Also:

Anhydrous Acids and Lewis Acids

Lewis acids are those which cannot provide a proton to another molecule but clearly react with bases. Like the proton itself, they are clearly in need of electrons. Their love of electrons has resulted in their being called "electrophiles". Although we generally use the term "electrophile" when no H+ is involved, it is also correct to call protic acids "electrophiles"



AlCl3 and FeCl3

Aluminum chloride has a central aluminum atom which has only 6 electrons; like boron in the acidic BF3, it is very electron-deficient. It is one of the stronger and more common Lewis acids used in chemistry. In the presence of alkyl halides (tertiary best, of course) or acyl halides, it can remove the halide to generate a carbocation (why are they stable?) and AlCl4-. The carbocation will react with whatever is available, even add to an aromatic ring. With carbons that are less able to support a positive charge, the aluminum chloride just loosens the C-Cl bond enough to make the carbon positive enough to react with the aromatic ring (and to rearrange as if it were a carbocation). Aluminum chloride is a powerful dehydrating agent as well, although not very selective; partially hydrated (to reduce its acidity) it works very well as commercial dehydrating agent - the antiperspirant aluminum chlorhydrate.

Ferric chloride is the catalyst of choice for halogenating benzene rings. The reaction proceeds like that of alkyl halides with aluminum chloride, namely polarization to remove a halide to form FeCl4-, and thus generating Cl+. An easy way to do this reaction is just to add powdered iron to the reaction and an excess of halogen; the halogen oxidizes the Fe to FeX3 (where X could be other halogens as well) which then catalyzes the reaction.

ROH2+

All oxygen-containing organic compounds, like alcohols, behave as bases in the presence of concentrated aqueous acids or anhydrous Lewis acids. Depending on what else is present, the temperature and the acid concentration, alcohols can be converted to ethers (one water lost for two molecules of alcohol) or alkenes (one molecule of water lost per molecule of alcohol). When acid and alcohol are added to other oxygen-containing compounds like ketones and acids and esters, they share the proton in equilibrium. The protonation of the oxygen makes the carbonyl carbon more susceptible to attack by nucleophiles in each case; however, any nucleophile that you use must be no more basic than the alcohol or carbonyl compound or it will be protonated instead! If just the carbonyl compound, alcohol and acid are present, ketones and aldehydes undergo addition to produce hemiacetals and acetals, although they are easily converted back to the aldehyde or ketone in the presence of water in most cases. With esters, acids and acid chlorides, the final product of reaction with acid and alcohol is an ester (perhaps a different ester if you start with an ester) via an addition - elimination sequence.

HX (HCl, HBr, HI) and Substitutes

The hydrohalic acids are gases and thus the aqueous "concentrated" solutions are not very concentrated; conc HCl, for example, is 35% in water. The high vapor pressure of the gaseous acid over the solution makes these acids very dangerous to work with, because the chances of exposure to the lungs is quite high. They are exceptionally good at corroding metals (my personal hypothesis is that the high vapor pressure is responsible).

Although HX's can be used for substituting alcohols with halide X, all sorts of side reactions occur with tertiary and secondary alcohols (rearrangement and dehydration). Better methods for substitution are: thionyl chloride (SOCl2) or PCl3, and for secondary and tertiary, the Lucas reagent, which is HCl made more acidic and more chloride-rich by a high concentration of the Lewis acid ZnCl2 (the water is now overwhelmed). Conversion of a carboxylic acid to an acid chloride cannot be done with aqueous HCl (the more stable acid is favored), but must be done with anhydrous SOCl2 or PCl3.



Has anyone any knowledge of this route having been attempted in the literature?


Rhodium

  • Guest
Lucas
« Reply #13 on: February 06, 2004, 09:08:00 AM »
UTFSE for 'Lucas' and this comes up:

Post 435996

(WizardX: "Lucas Reagent", Stimulants)


You also knew something about the reaction 4-5 years ago:

Post 103487 (missing)

(dwarfer: "Re: Why Iodine sub instead of chlorine", Chemistry Discourse)
 ;)


WizardX

  • Guest
haloephedrine
« Reply #14 on: February 06, 2004, 12:26:00 PM »
methymouse


That might work, though it's a bit unclear to me how you iodinate without HI.





Use phosphorus triiodide, PI3, (or a mixture of iodine and phosphorus, red, yellow, or both) in Carbon disulphide, CS2



dwarfer

wiz: can it be chloro-ephedrine?

Yes! But the iodoephedrine has the best leaving group -I



wiz:  I guess the CaH2 would MAKE it a super dry ether: would having some water to generate the H2 be of value (with CaO made because of the molar excess of CaH2 {Rhode said the reaction proceeds thru CaO to Ca(OH)2 with a surplus of water only.

Would there be any advantage to pressure?




NO! & NO! Any water in the ether or if the haloephedrine is still in it's hydrate form, eg. haloephedrine.1/2 H2O will predominate the reaction with the CaH2


Organikum

  • Guest
Finkelstein Swap
« Reply #15 on: February 06, 2004, 01:25:00 PM »
Make your chloroephedrine and do a "Finkelstein Swap" to replace the Cl with I.

Dissolve the chloroephedrine (base) in dry acetone and add NaI - slightly over 1mol - heat and stirr until no more NaCl precipitates.
Filter NaCl out and gass. Voila, iodoephedrine.HCl and some chloroephedrine.HCL what doesnt matter for your following reduction.

The chloroephedrine.HCl may be converted into the base in situ before - good stirring will be essential - dont overbasify or this will kill your pfed

good luck.


dwarfer

  • Guest
Subject: Lucas Bookmark Reply Posted by: ...
« Reply #16 on: February 06, 2004, 10:27:00 PM »
Subject:  Lucas   Bookmark  Reply    
Posted by:  Rhodium (Chief Bee)


UTFSE for 'Lucas' and this comes up: WizardX: "Lucas Reagent" (Stimulants)

Yeah, that's the same as on Wiz's web site that I reffed.

You also knew something about the reaction 4-5 years ago: dwarfer: "Re: Why Iodine sub instead of chlorine
" (Chemistry Discourse) 

You are right, I did and do: but thought it appropriate
to acknowledge the gentleman who brought up "Lucas
Reagents" to begin with.



 
   
 haloephedrine     Reply    
Posted by:  WizardX (Wizard Master)
   to dwarfer: re the question "wiz: can it be chloro-ephedrine?"

Yes! But the iodoephedrine has the best leaving group -I

I am aware of that from out of the past, as indicated by
Rhodium:

my THOUGHT is that no matter if it is a "good" leaving group,
or relatively "poor", that Ca will slice it out
no problem, given the affinity.

dwarfer to wiz:  I guess the CaH2 would MAKE it a super dry ether: would having some water to generate the H2 be of value (with CaO made because of the molar excess of CaH2 {Rhode said the reaction proceeds thru CaO to Ca(OH)2 with a surplus of water only.[/i]

dwarfer asks Wiz:
Would there be any advantage to pressure?

wiz to dwarfinger:  NO! & NO! Any water in the ether or if the haloephedrine is still in it's hydrate form, eg. haloephedrine.1/2 H2O will predominate the reaction with the CaH2

  Please bear with me here:  if there is an excess of CaH2 to snatch up and react with the water, whether as hydrate or free water, just as it is used to dry solvents,
why is it an issue?  the excess AFTER drying the mix should
(in my demented mind) then go on to scarf the  halogen.

an excess beyond that would remain unreacted.

After completion, maybe drip in a few drops of water to
react the excess.  The np would have MA and that % of
ephedrine that did not get halogenated.  The MA could
be selectively steamed away from the ephedrine.

Orgies replacement protocol of the Cl to I is great,
but does not obviate the bottleneck, which is the
chlorination process itself.  Plus, if I'm right
the Ca is "strong enough" to get any halogen. Wait
I already hypothesized that..

The question remains, is it really worth it to
obtain HBr and ZnBr2?  Only if the conversion
is higher than the 75% or so, I presently think.

Thank you for your insight and consideration.
:)

Edited for readability


methymouse

  • Guest
Uhh
« Reply #17 on: February 08, 2004, 02:08:00 AM »
"Use phosphorus triiodide, PI3, (or a mixture of iodine and phosphorus, red, yellow, or both) in Carbon disulphide, CS2"

Hmm.  How does one get PI3?  One could either order it (enormously suspicious) or one could make it out of RP from matchbooks and I2.  Hmm.  Is there another way to make meth out of RP and I2?  I need to do more reading.

Refluxing chloro-ephedrine with KI should work, though.  I hadn't thought of that.


dwarfer

  • Guest
Wizard's correction of my 2nd error
« Reply #18 on: February 09, 2004, 10:48:00 PM »
Thank you for editing.

As Wiz pointed out, (privately)if there was water in the NP
with the FB when the CaH2 was added, the Ca(OH)2
made would compete with the desired reaction,
with the OH going back to the chloroephedrine making
ephedrine again, big whoop..


dwarfer

  • Guest
maybe a third error??
« Reply #19 on: February 09, 2004, 11:06:00 PM »

Post 486546

(WizardX: "Don't give up!", Stimulants)


dwarfer: Don't give up! Work along the line as such.
CaH2 + haloephedrine in a super dry ether.

CaH2 + 2 C6H5-CH(-I)-CH(-NHCH3)-CH3 ==[super dry ether]==> 2 C6H5-CH2-CH(-NHCH3)-CH3 + CaI2

 


=============================================

Wiz you stipulated a "super dry ether".  Can either benzene,
xylene. or naphtha be used?
====================


WizardX

  • Guest
Ether
« Reply #20 on: February 10, 2004, 04:12:00 AM »
H3CH-CH2-O-CH2-CH3 diethyl ether has a oxygen with two lone pairs of electrons. This gives the molecule a semi-polar charge because of atoms electronegativity charges. This helps in the solvent action with the CaH2 and haloephedrine.

tetrahydrofurane (oxolane) can be used?

SPISSHAK

  • Guest
RE: oxalane
« Reply #21 on: February 15, 2004, 01:46:00 AM »
From what I know THF is preferrable over ethoxyethane in this regard because the lone pairs on the oxygen are much less sterically hindered than in diethylether giving a much better solvating effect.

Urban_XTC

  • Guest
reduction of Ephedrine via SOCl2 w H2 as catalyst
« Reply #22 on: October 13, 2004, 10:43:00 AM »

dwarfer

  • Guest
A REAL LIVE Failure! YeS!
« Reply #23 on: October 14, 2004, 03:37:00 AM »
8) Marvilous Marvin,
stimulated by possibilities,
entranced with dreams,
motivated by hope,
and positively full 0f imagry of the
wonderful contribution he was about to make
to ALL of Mankind:
(parTICKUlarly hisownselfness,)

did approximately the following,
as well as I could see thru the
40X looking glass,
and after decipherig his screams of rage,
an plaintive sobs of self-pity,
after the fool flubbed the deal...

=================



So anyway, looks like he took 6.5 grams of
 fake ephedrine (pseudo) and put it in a
250 ML beaker and was intent on adding the
'zact amount of ZnCl2 and HCl
to chlorinate the
6.5 grams,
but upon opening his
tightly-close bottle of ZnCl2,
discovered that the hygroscopic nature
of the material had confounded the HDPE plastic
and slurped enough H2O thru some ?? tiny orifices
to make your basic (<<anti pun..) :)
 unmeasured thick viscous
35% HCl brown solution
and the underlying undissolved
but damn solid mass
a real pain in the ass to deal with .

As a matter of fact, after seeing the guy trying
to pry some out with various tools,
I watched him finall go to his drill press
and drill some out.

So an unknown amount of Lewis acid blend was
poured on top of the huge pile of crystals
in the beaker.  It didn't dissolve it:
not by a long shot..

A watch glass was put atop the beaker to
minimize splattering..

The beaker was put in a glass measuring cup.

The measuring cup was put inside a large
sealable plastic kitchen-leftover type bag.

The large sealable plastic kitchen-leftover
type bag was put in the microwave.

The microwave was turned on, and the mass was seen
to dissolve into a viscous brown liquid.

the time of irradiation was about 2.5 minutes total:
each time the material was seen to begin to boil,
it was shut off and allowed to cool
for 15 seconds or so.

The bag began to swell, and Marvey,
who has trashed several microwaves,
decided to not trash his latest, and took the
bag, cup, beaker, and liquid outside to cool.

After it had done so, it appears that he
added some cheap-o $8/gal hardware store
alcohols, which is predominantly methyl:
with ethyl mostly # 2, but it varies.

surprisingly dry, it has been found..

He washed the material
in about three 150 ML quantities.,
and filtered it.

He mixed the alcohol with xylene,
and placed it on a stirring hot plate. 
As the mixture stirred, he added small  pieces of
CaH2, and did so as the temperature rose,
with copius H2 outgassing.

At the elimination of all alcohols at around 90C,
the hydride reaction became almost negligible.

The liquid was cooled, and filtered.

As  the .HCl and the Cl were eliminated from the
target molecule, forming an insoluble salt, the
now methamphetamine freebase
became intrained in the
Xylene, where, after gassing, it yielded the most beauteous
desoxyphedrine ever you have seen.!!!


this of course, was what the
loathsome Marvin had dreamed in
his vacant head:

and the absence of such a result
was the proximate cause for the
pitiful wailing, caterwauling, and cursing
which subsequently eventuated.

No, the poor dumb fuck got a cloudy white
broken-moleculed mess of extremely small particulate
chunks of god knows what but it wasn't what he was looking for.  .HCl salt chunks of it..  elsuckamundomucho

Pretty funny: you would think
he would come to realize that
what he thinks is going to be really suPERB
has likely already been thought about
by somebody who
may actually know what they are doing:

and generally dismissed outright as stupid.

;) Oh well: he seems to have fun in his fantasies.

and it's sure fun watching the poor bastard
carry on like that..

  i think likely the microwave treatment raises the
effectiveness of the chlorination so much that the
molecule has Chlorides sticking out in all directions,
and when the calcium  comes up it just rips the shit
outada molly-cule.

Isn't that good chemist talk?
 "rips the shit outa da 'cule."?? ;D

===================

Maybe somebuddy else has anudder idear??

Maybe a weaker Lewis combo oughta be used??

Howzabout Calcium chloride?

or maybe just 30 seconds at boiling?

who knows.. ::)
:P  


For real chemists doing real things:
see

https://www.thevespiary.org/rhodium/Rhodium/chemistry/ephedrine.catalytic.html



For nifty models of alcohols, see

http://people.ouc.bc.ca/woodcock/molecule/