Author Topic: Toluene Extraction The Final Frontier  (Read 4755 times)

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icecream_man

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Toluene Extraction The Final Frontier
« on: December 27, 2003, 10:06:00 PM »
Please don't flame me. I've been reading and researching the board for several months and this is my first posting. I went through the trials and failures of pill extraction until i finally got it right. I hypathetically got ahold of RP. Hypathetically I got iodine crystals from an online shopping service. If I wanted to give several friends really cool late XMAS presents and were to use below information from my research. It all makes sense except one step. It would be appreicated if someone could either make it clear or push me to a thread to research it better:


To do the reaction, a 1000 ml round bottom flask is filled with 150 grams of ephedrine hydrochloride (or PPA-HCl). The use of the sulfate salt is unacceptable because HI reduces the sulfate ion, so this interferes with the reaction. Also added to the flask are 40 grams of red phosphorus and 340 ml of 47% hydroiodic acid. This same acid and red phosphorus mixture can be prepared from adding 150 grams of iodine crystals to 150 grams of red phosphorus in 300 ml of water. This should produce the strong hydroiodic acid solution needed. Exactly how strong the acid needs to be, I can't say . I can tell you that experiments have shown that one molar HI is ineffective at reducing ephedrine to meth. The 47% acid mentioned above is a little over 3.5 molar. I would think that so long as one is over 3 molar acid, the reaction will work.

With the ingredients mixed together in the flask, a condenser is attached to the flask, and the mixture is boiled for one day. This length of time is needed for best yields and highest octane numbers on the product. While it is cooking, the mixture is quite red and messy looking from the red phosphorus floating around in it.

When one day of boiling under reflux is up, the flask is allowed to cool, then it is diluted with an equal volume of water. Next, the red phosphorus is filtered out. A series of doubled up coffee filters will work to get out all the red phosphorus, but real filter paper is better. The filtered solution should look a golden color. A red color may indicate that all the phosphorus is not yet out. If so, it is filtered again. The filtered-out phosphorus can be saved for use in the next batch. If filtering does not remove the red color, there may be iodine floating around the solution. It can be removed by adding a few dashes of sodium bisulfate or sodium thiosulfate.

The next step in processing the batch is to neutralize the acid. A strong lye solution is mixed up and added to the batch with shaking until the batch is strongly basic. This brings the meth out as liquid free base floating on top of the water. The strongly basic solution is shaken vigorously to ensure that all the meth has been converted to the free base.

With free base meth now obtained, the next step, as usual, is to form the crystalline hydrochloride salt of meth. To do this, a few hundred mls of toluene is added to the batch, and the meth free base extracted out as usual. If the chemist's cooking has been careful, the color of the toluene extract will be clear to pale yellow. If this is the case, the product is sufficiently pure to make nice white crystals just by bubbling dry HCl gas through the toluene extract as described in Chapter 5. If the toluene extract is darker colored, a distillation is called for to get pure meth free base. The procedure for that is also described in Chapter 5. The yield of pure methamphetamine hydrochloride should be from 100 to 110 grams.

The only part confusing me and it could be the fact I've been reading threads for 18 hours and is all running together is the final toluene extraction. Is there a thread that explains this step by step or could someone give me a little push in the right direction. Finally is this formula sound? Will it work?  Thanks and I've got my gasoline drawers on so please no flaming


livid

  • Guest
well to start with, your flask is to small for
« Reply #1 on: December 27, 2003, 10:16:00 PM »
well to start with, your flask is to small for that sudo number.

kris_1108

  • Guest
The Perfect Explanation
« Reply #2 on: December 27, 2003, 11:45:00 PM »
Hi
Read this

Post 428410

(geezmeister: "The post-reaction workup: a cook's summary", Stimulants)
Its a post reaction workup by Geez, and it is very informative. Read the whole thing - there are some posts there by Osmium which are also very helpful.
Then you are ready to GO!
Also read around at www.rhodium.ws/chemistry/index.html under "HI/P reduction of ephedrine" to learn of slightly alternative methods. Also see

https://www.thevespiary.org/rhodium/Rhodium/crystalcreations/index.html


and

https://www.thevespiary.org/rhodium/Rhodium/worlock/toc.html


for more reading material.
If this is your first rxn (reaction), and its gonna be ONE HUNDRED AND FIFTY GRAMS(!!!), then you would want to make sure there is little room for error. :)

Flask size - I think the general rule is 1ltr per ounce of ephedrine, so for you a 5000mL flask would be closer to the mark. (for 150gms).

-EDIT-
Just found out from a PM that 1ltr per 2oz should be ok...

adroit_synth

  • Guest
try one ounce
« Reply #3 on: December 28, 2003, 08:01:00 AM »
Rather than buy a new flask, just use an ounce of pseudo or you can make it a cool 30 grams but SWIM wouldnt go over 30g for a 1L flask. The final toluene extraction is simple, just shake toluene with filtered and basified RxN mixture, use a seperatory funnel to seperate the non-polar (toluene and free base) layer. Then gas it for pretty crystals! Filter em out and let dry (under vacuum if time or thoroughness is a concern). You might want to look into making some hypophosphorous acid and performing the reduction with that as it is a much easier/cleaner method. The red phosphorous can be a bit troublesome to clean up as most clandestine chemists have nothing that will dissolve it.


SHORTY

  • Guest
What?
« Reply #4 on: December 28, 2003, 09:02:00 AM »
The red phosphorous can be a bit troublesome to clean up as most clandestine chemists have nothing that will dissolve it.
Why would you want to dissolve the rp?


Rhodium

  • Guest
RP isn't soluble in anything
« Reply #5 on: December 28, 2003, 10:13:00 AM »
Why would you want to dissolve the rp?

Because recrystallization is great to purify compounds. But let's not talk about that anymore, as RP isn't soluble in anything.


SHORTY

  • Guest
What about phosphorus tribromide?
« Reply #6 on: December 28, 2003, 11:34:00 AM »
I read that it is soluble in phosphorus tribromide what ever that is.

I was trying to understand why he was saying that the hypo method is better since rp cannot be dissolved.  Whats wrong with filtering it out after the rxn is completed.  Its a little extra work but its not worth trying to obtain the hypo if you already have rp.  If you don't have rp then its well worth it though.


lugh

  • Guest
Solubility of Red Phosphorus
« Reply #7 on: December 28, 2003, 12:15:00 PM »
The CRC Handbook listing for red phosphorus states that it's soluble in absolute alcohol, ether and ammonia; and insoluble in carbon disulphide, in contrast to white phosphorus  ;)


adroit_synth

  • Guest
RP
« Reply #8 on: December 28, 2003, 09:20:00 PM »
SWIM clearly has no idea what RP is soluble in at this point for he has read so much conflicting data. He was under the impression that anything a clandestine chemist would have on hand would not suffice for dissolution and not much in a real lab would either. Elder bees have led him to that conclusion, and on the same note other elder bees have argued with them. I picked a side b/c SWIM knows he sure as fuck can't dissolve the nasty shit worth a damn. Sticks to nalgene and stays too.

Could be wrong, but my point wasn't that the hypo is better b/c of the insoubility of RP. It is better regardless AFAIK. Just an easier and cleaner synth. Of course the best synth is always goin to be a subjective matter, just MHO. By all means if RP is in hand, use it, just tryin to save a fellow bee a headache in future runs and myself from reading more glass cleaning posts.

a_s


adroit_synth

  • Guest
misinforming
« Reply #9 on: January 06, 2004, 11:04:00 AM »

lugh

  • Guest
Page from CRC Handbook of Physics and Chemistry
« Reply #10 on: January 06, 2004, 04:53:00 PM »
Here's the page from CRC Handbook of Physics and Chemistry that you seem to feel is in error  ::)




SHORTY

  • Guest
Allotropes of Phosphorus
« Reply #11 on: January 06, 2004, 08:48:00 PM »
Are any other bees able to see the pic in the previous post?

What is absolute alcohol? 

Would methanol, ethanol or iso qualify as absolute alcohol?

Everything i have found says the opposite. For example:

Allotropes of Phosphorus

White phosphorus is a soft, wax like solid, exceedingly poisonous and very reactive chemically. It ignites spontaneously in air. White phosphorus is soluble in carbon disulfide but insoluble in water, and so it can be stored under water. Red phosphorus does not oxidize rapidly at room temperature, although it burns very readily if it is heated sufficiently. Red phosphorus is much less poisonous than yellow phosphorus, and it is insoluble in carbon disulfide. These marked differences in properties between the allotropes suggest a difference in molecular structure.

A phosphorus atom has five valence electrons and its electronic symbol is usually written as P The molecular weight of phosphorus, as determined experimentally from its vapour density, is 124. Therefore, phosphorus vapour consists of P4 molecules. These molecules have an unusual tetrahedral shape, in which the four atoms are located at the corners of a regular tetrahedron.  In contrast to nitrogen which forms N2 in the gas phase with a triple bond, phosphorus forms P4 which has four strained single bonds. (At least this is true below 800 C; above this temperature the vapour consists of P2 molecules.)This is consistent with the known weaker double bond versus single bond strength on going down the periodic table. Indeed, compounds possessing stable P=P bonds were unknown until 1981.

Phosphorus vapour condenses to a liquid at 280 C and then to a solid at 40C.  The attractive forces between the molecules are van der Waals forces.  If the solid or liquid is heated, the P4 molecules separate and the vapour is formed.  From this we conclude that the covalent bonds which bind atoms into molecules are generally stronger than the van der Waals forces which bind molecules into a liquid or solid.

Black phosphorus is a crystalline network solid. White phosphorus is a non polar substance and, like rhombic sulfur, it will dissolve in non polar liquids such as carbon disulfide and carbon tetrachloride, but not in water.   Red phosphorus is amorphous rather than crystalline. It is therefore much harder to obtain the detailed structure of this solid, since crystallographic methods cannot be used. The structure of red phosphorus is thought to be chains of ring-opened P4 cages. It is prepared from white phosphorus by heating in the absence of oxygen at atmospheric pressure.  This thermal activation allows the ring-opening polymerization reaction to occur.  As one might expect, red phosphorus is the more stable allotrope; it does not oxidize in air at ordinary temperatures nor does it dissolve in non polar liquids such as carbon disulfide. If red phosphorus is heated to a sufficiently high temperature, the bonds between the atoms are broken and, on cooling, P4 molecules are formed which condense to the liquid and solid forms of white phosphorus.



lugh

  • Guest
Ethanol
« Reply #12 on: January 07, 2004, 05:35:00 AM »
Absolute alcohol is pure ethanol, a preparation can be found in Vogel's  ;)  The way that page is laid out is confusing, it's possible that it's stating that red phosphorus in insoluble in ether and ammonia, as well as carbon disulphide  ::)  Ethanol's hydroxyl groups make it a polar solvent, and there's little doubt that it's not easily available due to it's high cost and difficulty in getting it and keeping it dry  :P


SHORTY

  • Guest
Yeah i you got it mixed up...
« Reply #13 on: January 07, 2004, 06:04:00 AM »
Cause i know for a fact that ethanol will not dissolve rp cause i have used it to remove rp from strikers. 

I still can't see that file you posted.  Do i need to have a particular program to see it or should it bee visible on the page.  When i click on it i get a new window with nothing in it.

I did find about 8 different sites that were similar to the one i posted so i am pretty sure its correct.


lugh

  • Guest
Acrobat Reader
« Reply #14 on: January 07, 2004, 01:01:00 PM »
That's a pdf file, it should open with Acrobat Reader, as it does for others  ;)  I'm not confused about anything, it doesn't surprise me that once again the recorded facts of well known chemical publications would be disputed in this forum  ;D  You probably dissolved some of your RP in the ethanol, just not all of it, note the actual solubility isn't recorded. SWIL can't test this presently, as one would need both the anhydrous absolute ethanol and pure red phosphorus to determine the facts, and SWIL ohly possesses the former item  :P  Here's the page in jpg format:




SHORTY

  • Guest
From the Merck Index
« Reply #15 on: January 07, 2004, 09:23:00 PM »
From the Merck Index
Phosphorus

atomic no. 15, atomic wt. 30.975, non-metal, row 4, col 5A, val. 3-5, orbits 2-8-5

{Merck Index - © 1952 by Merck & Co., Inc.}

Phosphorus. P; at. wt. 30.975; at. no. 15; valence 3-5. Discovered in 1669 by Brandt. Does not occur free in nature; found in form of phosphates in the minerals chlorapatite, fluorapatite, vivianite, wavelite, and "phosphate rock" (S. Carolina, Florida, Tennessee); occurs in small quantities in granite rocks; occurs in all fertile soil; an essential constituent of protoplasm, nervous tissue, and bones. Prepn. Ullmann, Enzyklopädie der Technischen Chemie 8, 362 (1931); DeWitt, Skolnik, J. Am. Chem. Sec. 68, 2305 (1946); Skolnik, Tarbutton, Bergman, ibid. 2310.

Phosphorus exists in three allotropic forms: white, black, and red.

White phosphorus: Colorless or yellowish, transparent, crystalline solid; darkens on exposure to light; m. 44.1° (vapor press. 0.181 mm.); b. 280° d. 1.83; volatile; sublimes in vacuo. at ordinary temperature when exposed to light. When exposed to air in the dark, emits a greenish light and gives off white fumes. Almost insoluble in water (one part in 300,000 parts of water); very slightly soluble in abs. alcohol (1 g./ 400 ml.); slightly sol. in abs. ether (1 g./ 102 ml.); soluble in chloroform (1 g./ 40 ml.); soluble in benzene (1 g./ 35 ml.); very soluble in carbon disulfide (1 g./ O.8 ml.).
Solubility in oils: one gram phosphorus dissolves in 80 ml. olive oil, 60 ml. oil of turpentine, about 100 ml. almond oil.
Ignites at about 30° in moist air; the ignition temperature is higher when the air is dry.

Caution: Handle with forceps. Keep under water.

The fumes and the element itself are poisonous. Combines directly with the halogens to form tri- or pent halides; combines with sulfur to form sulfides. Reacts with several metals to form phosphides.  Yields orthophosphoric acid when treated with nitric acid.  Reacts with alkali hydroxides with formation of phosphine and sodium hypophosphite.

Incompat. Sulfur, iodine, oil of turpentine, potassium chlorate.

Use: Mannf. rat poisons; for smoke screens, gas analysis.

Black phosphorus: Crystals; resembles graphite in texture; produced from the white modification under high pressures: Bridgman,. J. Am. Chem. Sec. 36, 1344 (1914); Jacobs, J. Chem. Phys. 5, 945 (1937). d. 2.691. Does not catch fire spontaneously. Insoluble in organic solvents.

Red phosphorus: Red to violet powder; polymorphism: Roth, DeWitt, Smith, J. Am. Chem. Sec. 69, 2881 (1947). Its properties are intermediate between those of the white and black forms. Sublimes at 416°, triple point 589.5° under 43.1 atm. d. 2.34. Insoluble in orgamc solvents. Soluble in phosphorus tribromide. Less active than the white form; reacts only at high temperatures. Yields the white modification when distilled at 290°. Catches fire when heated in air to about 260° and burns with formation of the pentoxide. Burns when heated in an atmosphere of chlorine.

Caution: Avoid contact with KClO3, KMnO4, peroxides and other oxidizing agents because with these explosions may result on contact or friction.

Use: (Red phosphorus): Pyrotechnics; manuf. safety matches; in organic synthesis; manuf. phosphoric acid, phosphine, phosphoric anhydride, phosphorus pentachloride, phos phorus trichloride; raanuf. fertilizers, pesticides, incendiary shells, smoke bombs, tracer bullets.

Toxicity: (White phosphorus): Ingestion produces severe G.I. irritation, bloody diarrhea, liver damage, skin eruptions, hematuria, collapse, coma, convulsions. Extern. causes severe burns.


Jacked

  • Guest
reply
« Reply #16 on: January 08, 2004, 06:37:00 PM »

Flask size - I think the general rule is 1ltr per ounce of ephedrine, so for you a 5000mL flask would be closer to the mark. (for 150gms)




Swim runs 200 in a 3L flat bottom without a problem,
A 150gram run can be done in a 2L easy... 5L flask
you could get away with 400gram starts




SHORTY

  • Guest
I agree with jacked
« Reply #17 on: January 08, 2004, 09:19:00 PM »
I do 20-30g rxns in a 250ml without any problems.  I can't imagine doing a 30g in a 1000ml flask.  Hell i don't even have one that big.


livid

  • Guest
re: flask size
« Reply #18 on: January 08, 2004, 09:48:00 PM »
I hear alot of bees say; 1000 ml per 30 gram rxn, but when swim was a little kid, he saw the bikers doing 2 oz. rxns in 1000 ml flasks all the time, so I know it can bee done. They did it hot,dry,and fast, almost like the push-pull. the only thing diferent was, instead of the tube running to a push-pull, they ran the hose outside, stinking up the neighborhood

biotechdude

  • Guest
flask size for other methods?
« Reply #19 on: January 09, 2004, 01:14:00 AM »
I assume these flask size recommendations are for HI rxns using Iodine and (RP, HypoP, Pacid) that produce HI insitu.

Swix uses premade 57% HI, so he assumes that the flask size ratio would be different.  Eg as long as the flask is not over 2/3rds full with solution and with adequate condenser; it should be ok?