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METHCATHINONE   via     K2Cr2O7

By XplosiveKemistry

Cleaning Ephedrine

Several methods exist for the cleaning of pseudo-ephedrine, for thoroughness I will note "The Cure", written by the great Ozbee himself, which is a very detailed and preferred way to extract the pseudo-ephedrine from pills.

I recommend highly using a cleaner extraction method than the one I present here, but this will work in a pinch!

Start off by using any number of pills (use at least enough to make it worth while, but I've used as little as 2 gm). Make sure the pills don't contain acetaminophen (Tylenol), povidone, or guafinesin, as these will surely spoil the synthesis! These were cleaned in a very fast manner, again, may not be advised, to obtain optimum yields.

I started with 1440 pills of pseudo-ephedrine and placed in a wire mesh and put in an equal 'volume' of crushed ice. The cold, abrasive nature of the ice will remove the red coating and minimize the water erosion of pseudo-ephedrine from the pills. It is also acceptable to slowly trickle distilled water over the pill bunch to further remove the red, but take caution: excessive d-H2O will drop yields due to minimal loss of pseudo-ephedrine, so take it easy Once pills are cleaned in this manner, place in a 500 ml flask and add 200 ml of d-H2O. Place in microwave and let 'cook' ONLY UNTIL CONTENTS ARE HOT TO TOUCH, BUT NOT BOILING! This is one of only three critical points, so take care to do this properly. When this is finished, let the filler material settle and prepare the vacuum filtration. Liquid will still have a pink tint to it if cleaned as I did, but this is no big deal. Either decant this liquid slowly as not to disturb the gakk settled in the bottom, or can pour it all in the filter and clog it all to hell.

This WILL work, however, but you will probably spend more time scraping residue from the filter and waiting for it to finish than anything else, so my suggestion would be to decant, only a small amount of residue will fall into the filter and it will not need to be scraped for reuse unless using a smaller amount of pseudo-ephedrine. Repeat this procedure 3-4 times, or until the filler residue is no longer bitter. In any event, make sure the glassware will sustain the volume of liquid, as you will have double this amount of volume at the free base/extraction stage later on. Place this in a 1000-ml flask and put on a stir plate; drop in small stir bar and let stir.

Oxidation

Dissolve the ephedrine in water using this formula
under 1 oz -- use 30ml per 1gm of E
over 1 oz -- 250mls (initially)  + 25mls per 1 gm of E used over 28 gms
Measure out 0.5 gm of K2Cr2O7 (potassium dichromate) to every 1.0 gm of pseudo-ephedrine. Add dichromate while stirring the pseudo-ephedrine and let settle as much as you can while it’s stirring. Liquid will turn a bright orange color as the dichromate is added.
*(NOTE: NO coldness was needed in this process so far, but get ready, it’s coming.)
After making sure all of the dichromate particulate has indeed dissolved, slowly add sulfuric acid (98%) at 3 ml per 1 gm of pseudo-ephedrine. This brings us to the second critical point: Add this H2SO4 SLOWLY, as adding too fast will concentrate acid and it destroys pseudo-ephedrine, so go slowly or lose product! The orange solution will now start to get a dark color as the reaction takes place. On larger batches, if foam up starts, simply remove flask from stir plate and let settle, or help settle it with a glass rod or a STAINLESS STEEL butter knife. All you are trying to do here is settle the foam down and not panic. Easy problem, easy solution! Upon completion of adding acid, (liquid will be slightly warm, almost hot during this entire addition of acid stage, so it's OK) let this solution do it’s thing for 45-60 min. You will not want to go less than 45 minutes. Because I really don't think it gives the reaction time to take place, although, I've never been patient enough to go over 60 minutes.

This would be a really good time to grab a smoke/ drink/ whatever.
While the oxidation reduction reaction is stirring for this hour or so, you can do some other things to prepare the rest of the process,

Preparation of the lye solution

Red Devil lye was used here, 100 gm NaOH was slow dissolved in 400 ml of d-H2O. **DO THIS SLOWLY, ADDING THE LYE IN 25 gm INCREMENTS, and ALLOWING IT TO DISSOLVE AND COOL TO THE TOUCH BEFORE ADDING MORE. If you cannot do this slowly, you will most probably burst the flask due to either thermal shock or superheating it to the point that you can no longer hold onto it, thus dropping it on the awaiting feet below, so you may want to consider placing the water in an ice bath BEFORE you add the lye so as to avoid the whole thermal shock thing. Remember that you have a whole hour to do this, so take your time.

Slow down reaction use ice

After 60 minutes the oxidation reaction time is up. Remove the stir bar, and place the whole flask into an ice bath. This is our third and last critical point: Notice this is the first time ice has been used on the reaction solution. Let the reaction mixture chill for 30 minutes. or so to stop the oxidization and to insure that no thermal threats will occur, as you do not want this oxidizer/acid solution pouring from a cracked flask and on to anything that may be attached to you.

Freebase

Add lye Chromate Turns Green

Upon the completion of the 30-minute chill time, slowly pour the d-H2O/ lye mix (which should now be clear and slightly warm--maybe more than slightly, depending on how recently you made it) slowly to the oxidizer mix. You should at this time notice wisps of smoke coming from the mix. Relax, it's normal. You are looking for the mix to turn pale greenish. If it doesn't turn after all the aqueous lye solution is added, simply add more lye, although it is not necessary to dissolve it in d-H2O this time, simply pour it in slowly (think: teaspoon at a time) until it does turn green. You will start to smell the characteristic ‘pistachio’ smell, but be careful if the reaction goes back to a dark color, you will have burned the product. I don't know why this is, but YIELDS WILL SUFFER. Pour off a little of the base and test the pH, it should be at pH-12.5+, if not, add more lye at VERY SMALL increments--remember, you don't want to over gasify. I've had luck pulling a base of pH-11 or so, but the yield wasn't great.

The Goods

At this point, you will be enticed by the great smell of the pistachio, but never fear this is about to end! As soon as you get the base pH right, you may then remove this from the ice. Pour into the base about 300 ml of a non-polar of choice: Toluene, works best but availability may be limited Xylene, dries a little slower than toluene, but works the same Coleman’s camp fuel, always an option but any source of Naphtha will work in a pinch situation *Naphtha seems to leave an oily residue in the free base that isn't easily dried out when the CAT becomes an HCl-salt, so use it if it's the only thing you can find. Agitate this Toluene-base mix and let settle. The Toluene will rise to the top with the CAT free base in it. It will be an off clear to yellowish pale color. Decant this Toluene layer into a separatory funnel. You can do this twice cleanly but the third extraction will most likely yield nothing worth the time and effort. Do not allow any of the sludge to enter Sep funnel, pour only the Toluene into it, as this contains the product.

Make CAT water soluble

Add diluted HCl/d-H2O mixture to this...I used a 10% mixture and adjusted the pH as needed. My solution was 100 ml of 32% muriatic acid in 1000 ml of d-H2O that was prepared beforehand. ! You will see the water/acid/CAT fall to the bottom after you shake a few times, let this settle shortly You will be looking for a pH below 7.0 Then drain off water/acid/CAT into a beaker of appropriate size. Place on an electric stove with low to medium heat, or if you have one, place on a heating element not to exceed 150 F in either case. Let this heat until liquid turns a pale amber color or has evaporated 1/2 of the fluid away.

Microcrystals with acetone

Addition of some Acetone will form micro-crystals. These will be barely visible sized crystals and there won't be many, keep boiling and adding a little acetone looking for the crystals. We ain't done yet! When crystals begin to form Place in flask and seal with correct size stopper. Place this in the freezer for about 15-30 minutes. checking periodically to insure coldness, but not to the point of freezing!!! When chilled sufficiently, flood flask with ices cold Acetone (when the Acetone fills to the bottom part of the neck on the flask, this will be good enough). Shake vigorously for a few seconds and watch the crystals form and settle in the flask. This is the CAT in a soon to be consumable form. Let all crystals settle and strain through 2 coffee filter.
 

Removing the NaCl

Consistency of dried, uncut CAT will be slightly rocky, but otherwise like powdered sugar. Once the CAT has been produced and has been semi -dried, we need to remove nasty NaCl and other salts that appear in the final product. While still in the filter add some dry alcohol such as Methyl alcohol (Methanol) or Denatured alcohol. Dissolve as much of the dry CAT powder into denatured alcohol as is possible. (The (salt) NaCl will not dissolve) The filter traps unwanted salt Collect the liquid \Cat/Alcohol in and a clean flask or bowl. Bring the CAT/alcohol to a slow, soft boil. DO NOT LET THIS MIXTURE OVERHEAT! Keep a constant surveillance on this at all times and NEVER do this over an open flame or other source of ignition, use a warmer plate or a hot plate with a temp regulator.

Final re-crystallizing

As soon as some crystals form, seal the container up tightly and place in the freezer for approx. 8-12hrs for re crystallization. Pure CAT will slowly form; the crystals will be tight and clean. Filter the crystals to remove the alcohol. While in the filter lightly rinse away all alcohol and residue from the crystals with a splash of cold dry acetone. Let air dry, and enjoy!

Comments

Yield on this synthesis should be at 80% or higher, depending on how clean the pseudo-ephedrine is. One needs to exercise extreme caution that at no time a flame is introduced around Toluene, Denatured Alcohol, or Acetone, and the recommendation of some light rubber gloves would make acid handling safe. This synthesis was reconstructed for simplicity and consistency, as well as my own personal experience of trial by error. All elements here key off the use of pseudo-ephedrine in grams, NOT MILLIGRAMS, so adjust weight accordingly! None of these chemicals are on the highly dreaded watch list and most can be had right from hardware stores and Wal-Mart.

XplosiveKemistry
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