This file is a part of the Rhodium site archive. This Aug 2004 static snapshot is hosted by Erowid as of May 2005 and is not being updated. > > Back to Rhodium Archive Index > >
(PSEUDO)EPHEDRINE
REDUCTION WITH
I2
AND
H 2PO2
...Or "Go-Go without the Red - A tale of the Hypo Method" [ Back to the Che mi mistry stry Archive Archive ]
Disclaimer : The material contained herein herein is merely for informational purpose purpose and is not not to be carried carried out unless written permission from local law law enforcement is gained. The author tak es es NO responsibility responsibility for what one does with this information. Before even reading reading the procedure procedure below, below, check with your local/state/national government to ensure that the law is not being broken.
O VERVIEW Due to the diffi difficul culty ty in in some some area’s are a’s to acquire rp, SWIM S WIM went in search searc h of alternate alternate methods methods for Go-Go. Go- Go. (Well, (Well, and to try something something new). A post on o n Rhodium Rhodium’s ’s site done by Pebble Peb ble (Reduction (Reduction of Ephedrine to Methamphetamine Using Hypophosphorus Aci Acid d) with a few references refere nces on the hive hive where all that was found. After several sever al very very successful succe ssful reaction rea ction and amazed at the quality quality of end product pro duct it was determi de termined ned that more more info info was needed need ed out there. Pebbles Pebbles method had many concerns conce rns regardin regard ing g safety that were botherso bo thersome. me. (Smellin (Smelling g contents in between betwe en stages of the reaction. Reaction Reac tion being being carried carried out out in in an an open open vessel vessel,, ect…). Tha Thatt brin brings us to thi this poin point.
M ATERIALS: 7 g of P-fed P- fed or Eph…C Eph…CLEAN LEAN (E-Gull method, method, or The Cure on Cure on cleaning out the Gaak). 11 ml Con. Hypophosphorus Acid (Conc. Described later)
14 g I2 crystals (If tint is used, make sure that it is absolutely dry!) 1 : 1.25 (E : Hypo) & 1 : 1.5 (Hypo : I) 250 ml Flat Bottom Flask (or any reaction vessel) 200 ml beaker PYREX Evap Dish Reflux Condenser or 3 ft Surgical Tubing Heat source (Hot Plate or electric eye) d-H2O (Don’t risk loosing quality over 79 cents / gal) Sodium Hydroxide Ice (For Reflux Condenser Cooling and basifying) Sep Funnel (500 ml glass works great) Toluene, Naphtha or Non-Polar solvent of choice (Xylene has been the choice lately due to Gaak's solubility in Toluene) HCl (30% LG), or Muratic Acid if in a pinch 6- Pack of beer of choice
BRIEF NOTES: Don’t be sloppy The end result is directly proportional to the effort applied! Dry reagents are a necessity. Water in any of the Hypo/I/E will hinder the reaction. Take pride in your work, and don’t be in a hurry.
IN
TH E
BEGINNING
The E and Hypo are placed into the reaction flask
(250ml flat bottom or larger). Heat is genteelly applied to the flask. What your are looking for is the E mixing with the Hypo. Not all the E will mix, but get as much as possible. Place sealed flask in the freezer for 20- 30 min. (Hypo loves to absorb moisture) Set up the reflux condenser with ice water circulating through it. If no reflux is available connect tubing to a stopper of the appropriate size to fit the reaction flask. (Any which way, drink a beer). Remove the flask and place in a ice bath, acetone and ice works well fine. On rxn above 10g one may concider using Dry Ice and acetone for a ice bath.. (Keeping the contents cold will help buy you some time while connecting up the reflux condenser or tubing and will help keep the reaction under control). Attach tubing to the end of the reflux condenser, or flask if not using a condenser, and run it to your vapor containment unit (VCU, p/p unit, a bottle with the tube stuck inside and a wet paper towel to seal off the opening. The beer bottle from that beer you just drank could work). The I is added to the flask and spread over hypo/E as best as possible while the contents are still frozen. Once the I hits the Hypo/E mix and the flask and contents slowly warm, it will start to liquefy. (Sometimes one side of the flask is still frozen while the other is bubbling away). Bubbling will start to occur and will get more vigorous. Better yields and fewer side products are obtainable by allowing the reaction to liquefy, but not bubble out of control at first. ( DO NOT smell the fumes…They will raise hell with your nose and lungs ). The flask may have white smoke inside. Once liquefied, gently swirl the flask and mix the contents as best as possible. The color should go from dark red/purple to a light reddish-yellow. If the color didn’t change or the I2 is still liquid, gently swirling the reaction flask and place onto a WARM heat source. (Try using the palm of your hand first then a hot plate set on warm). If the contents of the flask have not gone to a orange-ish/reddish color after applying heat, then add 1 - 2ml of Hypo and mix gently. If your Hypo has been
have to be applied to boil off the excess water. Apply low-heat to the reaction flask until it starts to bubbling at a good hard steady rate. Note: DO NOT heat contents above 180° - 200° C or yields can suffer. Once a steady bubbling begins, look for white crystals (HI) in the tubing or in the glass tubing connector in the stopper. If a fog is forming in the vessel, try to keep it going for a few minuets. The contents should continue to bubble by itself for some time even when removed from the heat. (30 sec up to 4 min, depending on the vessels wall thickness and the Hypo/I amount). Look at the color of the reaction. If you notice a reddish color starting to appear, give the contents a few swirls and then place back on the heat. If the reddish color forms again, 1-2 ml Hypo should be added down the condenser/tubing and placed back on the heat. The color should lighten back up to a light gold/pale yellow color. Remove from heat.
After the boiling has subsided, mix/swirl the contents and then heat was again applied to the bottom of the flask. Notice the length in time decreases that it w ill boil by itself. Pay attention to the size of the bubbles in the solution while the contents are being heated. As the reaction goes on the size of the bubbles get larger . Note: Kee p the contents liquefied. To much mixing and letting the contents cool will cause it to solidify and is a pain to get it going again.
White smoke should have been noticed faintly flowing into the flask. Large amounts of 'snow' should be pressent on the glass walls. Add a few mls of dH2O down the tubing or reflux condencer to wash the 'snow' down. Return to the heat source. After 20 - 30 min of the smoke flowing into the reaction vessel, disconnect the tubing at the opposite end of the flask and add a few
more ml (1 to 2 ml MAX) of dH2O to assist in washing down the new 'snow'. Work the water down into the flask. You should start seeing more white smoke flowing into the vessel. Apply heat until the fog flow rate into the flask is clearly obvious and fairly constant. ( Usually let this run for another 10-15 min…Overkill? Don’t know, but one wants to make sure everything has been converted) Note : Check the temp of the reaction. Re member to not go above 180° C or yields can suffer. When the size of the bubbles is dramaticly larger than they originally where, the reaction is done. If unsure the reaction went, apply heat once again and notice if there is a change in bubble size and length of time it bubbles when removed. The color of the solution should now be a pale yellow to almost a clear color. If the bubbling dies off fairly quickly, its probably done. Un-stopper the flask. Now all the harsh nasty vapors should be undetectable. If experience has been done with the rp/I method you should be able to smell “That Smell”, if not experienced, there should be a sweat rotten-egg smell, but nothing that irritates your nose. If “The Smell” is undetectable, your not done. Place contents back onto the heat source and bring to a slow boil for 10 - 15 minutes (almost like refluxing), and then check again. Phase One completed.
A
L I G H T AT TH E E N D O F TH E TUNNEL
Continue washing down the walls of the flask, condenser/tubing with dH2O. Once satisfied, prepare 200 to 400 ml of your NP (Toluene, Naphtha, Xylene ect.) and place post-reaction vessel in a ice bath. (Whooooaaaa there little horsy!!! You didn’t filter it…No need to since you are not using rp. Put in CLEAN precursors, you get clean post reaction solution. A perk of this method over the rp’s, you get the goods without the crud). While contents are chilling, now is a great time for another beer and to clean up the equipment from phase one. With the NP and near Go-Go cooled, add your sodium hydroxide (aqueous solution or direct) in small amounts to the flask. NOTE: A solution is preferred over directly adding lye to contents due to less gaak noticed in the pull
process and less exothermic reaction. What one should be looking for is ’snow’ or the solution turning white to form and not clear up after several minutesLet the contents settle down again and mix/swirl flask. If the white went away, your not there, so add a bit more base. This process will keep one from adding more lye than needed and causing ‘Lye Lock’ from occurring. Keep adding your lye in small portions and swirling until the solution is ph 12.5+. If desired, pour in some salt to help push all the Go-Go up into the NP, but use NON-IONIZED!.
Decant the top layer into your sep funnel. Don’t worry if some of the bottom layer gets in, you want to get all of your NP though. Shake, swirl what ever for several minutes. Let settle then decant the bottom layer off and SAVE. Swirl the funnel to wash the side wall down. While the contents settle, drink a beer while you heat up 50 ml of dH2O in the microwave (for about 45 sec, or until it boils vigoursly). Drain off the bottom layer again if any. Pour in the hot dH2O into the sep. Swirl the sep around for a few seconds before placing the top on LOOSELY. (Vapors are produced when something is heated). Wash the NP layer well to rid it of any Gaak, contaminants and excess sodium ions. While contents are settling, finish the remainder of the open beer. Decant the bottom layer and add 50 - 100 ml of chilled dH2O. (About 1/2 the amount of NP). Swirl/mix/shake the contents. Let settle and then decant. Do this a few more times with hot then cold dH2O. After the final wash, let the sep settle for awhile. Drain off the bottom layer of water/Gaak if any. Swirl funnel to wash down the sidewalls and let settle. Drain again if needed. Add 30 – 40 ml of dH2O to the sep. Now add 4 – 6 drops of HCI. (Its actually about 6 drops/gram of expected Go-Go, but until you have the process down add the HCl in smaller portions to avoid possible problems until you are familiar with the process of A/B). Mix thoroughly by shaking or swirling vigoursly. Let settle and check the pH of the bottom layer. If using pool/spa test strips, note the Total Alkalinity. As this number gets closer to the OK range, it will take less and less HCI to lower the pH. (Some may say that is all that needs to be done is drop the pH down the first time and follow up with Acetone Crashing. It doesn’t make much difference, just preference). Add more HCI, mix, and check again. If slowly adjusting the pH bit by bit, once the pH is 7.0 to 7.3, place this liquid in the PYREX pan and the pan on the hot plate turned on low, to be dried. If Acetone Crashing was done, pour off excess acetone (and save) then rinse all the GoGo again with chilled Acetone.
No matter what process was done in the above step, there is still one more step to be carried out for quality, purity and prideful reasons, known as Recrystallization. ( Hell, if no attention was paid to the disclaimer/warning then what is one more step going to matter. One may as well have the best Go-Go on Cell Block C )
R E C R Y S T A L L I Z A T I O N ( from Worlocks website: rxn1) Re-crystallization of chili using methanol, denatured alcohol, or 91% isopropyl alc. will grow some very pretty, large crystals and will make your product more pure and much more potent. This is one procedure that is simplicity itself and always produces a major improvement with surprisingly little loss of product.
Crystals, using denatured alc. and vision ware (Worlock)
After the chili was pulled out of the toluene (non-polar solution) using HCl and water, It was run through a filter and placed
These were crushed and washed with ice cold dry acetone. The washed Crystals were then dissolved in hot denatured alc. the alcohol was boiled away until the first sign of skin forming or the first sign of crystallization noted. Remove from the heat add enough alcohol to remove the skinning so no more crystallization can be seen then add 20 ml of acetone, if it turns cloudy add alcohol drop wise until it is clear again cover and place in freezer 6 hours or more( overnight is great) you will return to find crystals floating in the liquor. Rapidly filter out the cold crystals , then wash them with a little cold alcohol to remove any gaak on the surface and in the outer crystal layer, set out to dry.. All three steps were performed without ever removing the chili from the vision ware bowl.
Recrystallization details The Chili is dissolved in a minimum amount of dry alcohol, this is heated, USING a Safety fan (Always) as needed to get it to dissolve , bring it to a soft boil . Continue boiling until you begin to see the chili form crystals on the surface of the alcohol. Known as the Lynrd sign., (The Lynrd sign?? Skynrd?? The chili forms a surface skin it was a joke get it ?? Lynrd Skynrd!!!) This is a super saturated solution . Add a little alcohol to dissolve the skin again, and add 20 ml of acetone Then cover and set in freezer, as the temperature drops, crystals will form . Leave in freezer for 6 to 12 hours or even longer. Generally the longer in the freezer the bigger and better will be the crystals. The chili re-crystallizes as the temperature drops, the alcohol won't freeze. As time goes on the crystals "digest". Digestion means the crystals are slowly re- modeled, the outer layers with impurities are stripped away a reform without the impurities. In addition the smaller crystals dissolve and become incorporated into the larger crystals because of volume(cubic) versus surface area(square) considerations After which the resulting crystals were quickly cold filtered , washed with a little cold alcohol and dried. The crystals should be rinsed lightly with alcohol to wash off any of the mother liquor that is stuck to the crystals, and to remove the outer layer of crystal which is slightly impure for even better results: The super saturated solution(dissolved in hot solvent) forms crystals faster than the hot but more dilute solution , but the more dilute allows better digestion and more pure crystals. --Worlock—
Your now done…Take the final product and dispose of it into the toilet and flush. (In many places it is illegal to be in possession of drugs unless local law enforcement say its okay).
Picture of produc t after recrystal izing .
NOTES
E-GULL M
ETH O D
B Y : WAREAMI
AS
TAKEN
F R O M TH E
HIVE
…since the results were so favorable with the hy dro-chloro-fluoro carbon group. Somehow this involves the s ingle-double bond but s ince none of the researchers are true chemists...No amount of planning will ever replace dumb luck. WaredItGo set out in search of everything that co ntained the word ethane/ethy lene/chloro/fluoro.....etc...etc...blah blah! Well there is a p roduct th at was b rought back and tes ted th at was aqu ired at the au toparts sto re(several...as a matterafact)This produ ct is used in cleaning brakeparts.....it con tains tetrachloroethylene and Co2. WoooooooooooooHoooooooooo...WATTS that SMELL? Damn....feels like We're buzzin around the Dry-Cleaners. SQUEAKY CLEAN! Well....thare y a hav e it! Thare is s till room for invest igation and tes ting, but it is p retty s traightfoward an d SupER EasY! No A/B! No Water! No Elaborate s et-up! Humblebee didn't want me to post this cau se it may mean an end to t he p-fed as we know it. Stay-tuned for the procedure in Part Two of "Warediditallgoright?" Peace Have Fun-Bee Safe 1)using tetra...you need the pill mass to be completely in contact with the solution. If any does not dissolve in the treatment...it will go through and foil you in the en d. MAKE SURE you are crus hing you r pills thorou ghly to a fine powder....and soak.... 2)pour off the tetra using ONE!!!! filter to g et yer pill/p-fed mass. If you us e more than one filter....you will trap th e poly's in the p ill mass that you are keeping. SQUEEZE off the excess tetra liquid while it's in the filter...you will be left with a ball. 3)Now you have to break this mass up and allow to dry to rid the pill mass of the DryCleaning smell. 4)Then you dissolve in Alcohol of choice...This stage the pill mass/alc MUST be filtered very well allowing no cloudiness to pass through....If it's cloudy...you may be getting some plastics in the mix. The foiling polys are gone but the plastics/wax and shit is in yer pill mass. DONOT keep pu lling this pas t the PINWHEEL crys tal stage caus e you are pulling GAAK.....SWIW finds that a three t ime Alky Extract of the pill mas s g ives a 95% yeild! If this techn ique works on generic ACTAFOOL and ALLFEDUP(
Peace of the react ion Have FUN-Bee SAFE ANO
TH E R
WA Y
O F
CLEANING E
With many new curve balls that are being thrown at one these days as buffers/blockers in E, the following steps are a BARE-MINIMUM!!! Grind the pills in a coffee grinder until they are a fine powder. (Unless using 12 hr. These are placed inside a metal sifter which is then place into a bowl full of acetone. After several minutes the casings will split open. Shake the sifter and the insides fall down into the bowl and the shell are left behind to be disposed of). Take powder and place in a beaker large enough to hold 3 times vol of powder. Next pour 2X powder vol of Tolulene onto the powder and stir thoroughly. Do a 15 min boil. Decant and repeat one more time. Dry Complete ly (Hint: try not to power or stir up contents very much. When dry, run the poweder through the sifter again. This will remove more gaak that the Tolulene help extract). Do the same as above except with Acetone (Remember that Acetone boils BELOW 150° F, so think a little!) Repeat at least one more time. Drain off Acetone and dry completely! Once dry, pour 3X vol of alcohol of choice onto the pill mass and place in freezer for 20 – 30 min. Decant alc off through 3 coffee filters + a cotton ball stuffed into the bottom o the funnel into a drying pan and repeat 2 more times. Each pull reduce the amount of alc so as not to waste it. AC
ETO N E
CRASHING
--geezmeister— --No. 238802— It works similarly whether the pfed (or Go-Go) is dissolved in water or alcohol. Not quite the same, but similar. Water,in SWIG's experience, needs to be evaporated closer to dryness before flooding than alcohol does. Acetone crashing is not a substitute for evaporation as much as a last step. With alcohol,evaporate t o the point that the surfac e skins over but before t he surface "alligators" or greatly wrinkles u . Flood the alcohol with acetone all at once, at least enou h to cover the c ontents in the bowl
about 3 times it depth. (You can add acetone if you were evaporating too fast, the bowl is too hot, and too much ac etone boils off. ) T he ac etone will sizzle and boil like mad at first, t hen settle t o a steady boil as the bowl cools. During this time, swirling the hot acetone helps free any pfed (or Go-Go) stuck to t he bottom or sides. (If you evaporated t oo long, you will need to c rush any clumps of pfed in the hot ac tet one with a glass rod, a gloved finger, et c. ) When evaporating an water-pfed (or Go-Go) solution, SWIG lets it evaporate even more, until the skin is heavily alligatored and almost all of the water is gone. There will still be some fluid under the skin if the bowl is tilted, but not a lot. Heat should be reduced after the solutions skins over, but well before dryness. SWIG flashes before total dryness, but not m uch before. He tries to avoid tilting the bowl so much t hat the pfed (or Go-Go) c akes on the sides of t he bowl before flooding with acet one. If there is t oo muc h water remaining when the solution is flooded with acet one, some pfed ( or Go-Go) will remain dissolved in the water and the pfed (or Go-Go) that crashes out will be wet. These crystals will dissolve into a paste. Too much water will make filtering meaningless--as it cools, you will the have the same mess on eac h side of the filter. Both sides will have too m uch wat er st ill. You will have t o do it ov er. Add water to dissolve, evaporate again, flash again. Flashing is like tightening up a plumbing connection. There is a quarter of a turn between too loose and too tight. You have to develop a feel for when the solution is dry enough to flash, just like you have to have a feel for how tight is "tight enough." How dry your ac etone is, how c old it is, how hot your evaporating dish is, how dry you pfed (or Go-Go) solution is-- are all variables. Control as many as you c an for c onsistent results. Flashed with t he right amount of ac etone at the right dryness of the solution, you will get nic e white sparkly crystals of pfed (or Go-Go) and brownish, trashy acetone. Rinse the crystals with cold dry acetone to get any remaining acid or other trash out.
H YP O P H O S Q / A Q: SWIM has been using the hypophos method for the past while with great success until recently his
yields have suddenly dropped down to ~20% (Before > 70%). He was wondering if you might know
can do without having access to all the fancy lab equip.
A: Hypophosphorus acid, H3PO2 will reduce hot sulphuric acid H2SO4 to sulphur dioxide SO2 + sulphur S Heat a little sulphuric acid H2SO4 in a test tube and add this hot sulphuric acid H2SO4 with a pipettes to your warm Hypophosphorous ac id, H3PO2 solution. If you see sulphur formed (solution goes cloudy) and a s mell of sulphur dioxide SO2 then the acid is OK! --Wizard X--
Q: How does one raise the conc. of hypo? A: In the crystalmeth forum under free base hypo nano, geezmeister claims to have raised concentration from 50% to near 90% of hypo by boiling. Suppo sed ly 50% isn't enuff to reduce E… (Pour the hypo solution into a large beaker and place a candy therm. in the s olution. Place on a hot plate. Note the temp at which boiling initially occurs. After the boiling point has raised ~ 12° let the now concentrated solution cool. Preforming the concentration procedure under vacume is preferred due to less of a possibility of the hypo decomposing )
-- morpheus - -- Post No 238779—
Q: Is hypo more dangerous to work with vs. RP? A: Be damn careful heating the solution. Make sure you have that wet towel handy and have a proper fire extinguisher. If you do not believe me, be sure you have insurance. Do not breathe the fumes when it burns, friend. Notice I said when, not if. When you have fire belching from the push pull tank and fire blowing out the end of the hose, remember someone did tell you to have that towel handy. It isn't a matter of if, it is more like when.
--geezmeister ---No 238809—
Q: What are some hints that one should follow? A: Research, Research, Research and still more RESEARCH! Don’t be STUPID…Think before you do anything…Hope for the best, but plan for the worst case senerio. “ Loose Lips Sink Ships’ Keep your mouth shut about your doings and take your time gathering. You control the reaction, not it controlling you. Start with only the highest quality precursors that you are capable of… DON’T BE LAZY…HAVE SOME PRIDE! DO IT RIGHT! Observe EVERYTHING that goes on throughout the whole process. Know what is going on. Note what occurred in both successful and failed reactions. (Why not learn from the mistakes?) After the basics are down…Experiment and try new things like varaying the amount of precur’s, setup, run time ect. - - E X C E R P T
FROM
T H E H I V E
Congrats. Does seem remarkably easy, does it not? Things SWIG said to me about this synth: 1) Concentrate that hypo some. It works. Really does. Big difference. Diff between 50% and 80% returns. 2) UTFSE and read the posts on hypo. Look for the little pointers. 3) Be damn careful heating the solution. Make sure you have that wet towel handy and have a proper fire extinguisher. If you do not believe me, be sure you have insurance. Do not breathe the fumes when it burns, friend. Notice I said when, not if. When you have fire belching from the push pull tank and fire blowing out the end of the hose, remember someone did tell you to have that towel handy. It isn't a matter of if, it is more like when. 4) This synth needs very little, if any heat. SWIG has had 70% returns with minimal heating.
5) Dry iodine is a plus. Wet iodine is a minus. 6) Use an excess of hypo. Go 1.2 to 1 Hypo to E, maybe a little more. You will not need to add. 7) Add the iodine in intervals. (author’s note: if done in intervals, the reaction is opened up to the world and you are then exposed to is possible dangers. Do it all at once)Be patient. Wait for that finished smell. If that smell does not come and if the solution stays golden and not yellow, think about adding a little more hypo. You still have iodine present. 8) Yes, it is perfect for the nano cook. 9) You can blow it, get no return, or get lousy, half reacted dope. But you have to be sloppy to do it. 10) Yes, use naptha and kerplunk. It does improve the gear. Amazing? yes. One pull and you're done? Easy. 11) Isn't it nice to see stuff this clean and pretty at the start? No burn, very little rush. Pure go and get it done stuff. Smooth as it can be. No teeth ground down. Up for days. 12) Understand no one believes this synth works. Accept it. It really is a trade secret. 13) SWIG says he is keeping notes for a start to finish nano write up when he feels like he has this really down. He does maybe one a week. Wanna help the write-up? --geezmeister--- No 238809--
