AmphetaminesAmphetamine F.A.Q.Abstract: While no list is ever complete, this one attempts to answer technical questions related to the chemical methamphetamine and its synthesis, for more info see the booklist. Unfortunately, there tends to be a great deal of street lore that is blatantly wrong about methamphetamine and similar compounds. This document also attempts to point out some of the more common myths, and provide rational explanations. Disclaimer: Do not use this information. I am not a chemist. This is for informational purposes only. Use of this information for illegal purposes is not condoned. The author makes no warranty, expressed or implied, of the suitability of this information for any particular purpose. The author does not endorse the abuse of any drugs, legal or otherwise. This information has been gathered from openly available sources. This is a preliminary document and should be considered fictitious until proven otherwise. Overview: Methamphetamine (also known as speed, meth, crystal, crank, and sometimes confusingly called ice) is a chemical widely known for its stimulant properties on the human body. It is frequently confused with other drugs that share similar symptoms, including amphetamine, 4-methyl-aminorex, ephedrine, caffeine, and other chemicals, both legal and illegal. Terminology: In this document, we shall refer to the drugs by their common chemical names, rather than by street names, since the street names do not have a one-to-one correspondence to actual chemicals. For example, the term speed can mean methamphetamine or amphetamine. The term ice is generally considered to apply to 4-methyl-aminorex, but is often used to refer to relatively pure (and in some cases, not so pure) forms of methamphetamine. We shall use the term methamphetamine to refer to the substance in either its free base (i.e. simple, unadorned) or salt (usually hydrochloride) form. When precision is needed, we shall explicitly state one form or the other. PharmacologyThis is one of the most difficult sections to write, partially because there is very little science involved. The literature gives conflicting reports, due to the fact that many criterion are subjective, and probably also due to confusion over terminology. The pharmacological effects of methamphetamine are very similar to those of similarly structured molecules. Administration: Methamphetamine can be taken orally, snorted, smoked or injected, in approximately increasing order of immediacy of onset. Onset: Onset can be immediate (in the case of injection), or can take as long as 30-40 minutes if ingested orally. Duration: Duration is subjective, but is probably on the order of 4 - 8 hours. Delayed absorption (for example, due to oral ingestion) can prolong the effects relative to time of administration. Of course, larger doses last longer due to the fact that it is removed from the blood at a finite rate. Plasma Life: The length of time that methamphetamine will stay in the plasma (blood) is between 4 to 6 hours. It can be detected in the urine one hour after use and up to 48 hours after use. Dosage: A toxic reaction (or overdose) can occur at relatively low levels, 50 milligrams of pure drug for a non-tolerant user. Different peoples' metabolisms work at different rates, and drug strengths vary, so there is no way of stating a safe or unsafe level of use. Effects: These include euphoria, hyperexcitability, extreme nervousness, accelerated heartbeat, sweating, dizziness, restlessness, insomnia, tooth grinding, incessant talking, and other effects. Methamphetamine and other CNS stimulants have strong bronchodilation effects. Vasoconstriction (tightening of blood vessels) and pupil dilation are also common. Elevated blood pressure, heart rate, and other general symptoms of increased sympathetic nervous activity. The physical effects are almost assuredly due to interactions between the amphetamine structure and human physiology, probably due to the similarity to adrenaline (epinephrine). Mental capacity is not diminished directly by the drug. In fact, some studies have shown slight increases in mental capacity on simple tasks. It has been prescribed for attention deficit disorder, among other things. Confusing reports here tend to center around the effects of fatigue on mental capacity. Emotional responses may range from euphoria to anger and paranoia. Preliminary doses tend to produce the former, while continued use (e.g. for three or more days) tends to produce the latter. It appears that these feelings may be linked to the neurotransmitters dopamine and/or serotonin, although I have not seen a good reference on this yet. ChemistryThis is the easiest section to write, and the most fun, since I can be relatively sure of the facts. You will notice that the salt form is much more common. This is for physiological reasons. The same reaction which attracts the free base to HCl could also attract it to other molecules, causing irritation and other symptoms. Methamphetamine Synthesis From: lamontg@u.washington.edu (Lamont Granquist) Condensation Product of Phenylacetone and Methylamine From Ephedrine or Pseudoephedrine From: yshan@bcarh697.bnr.ca (Yogi Shan) Reduction With Hydroiodic Acid and Red Phosphorus Method 4: Reduction With Hydroiodic Acid and Red Phosphorus In this procedure, the alcohol grouping of ephedrine, pseudoephedrine, or PPA is reduced by boiling one of these compounds in a mixture of hydroiodic acid and red phosphorus. Hydroiodic acid works as a reducing agent because its dissociates at higher temperatures to iodine and hydrogen, which does the reducing. The dissociation is reversible. The equilibrium is shifted in favor of dissociation by adding red phosphorus to the mixture. The red phosphorus reacts with the iodine to produce PI3, which then further reacts with water to form phosphorus acid and more hydroiodic acid. Since the hydrogen atom of the HI is being absorbed by the ephedrine, the red phosphorus acts as a recycler. In some reductions, the need for HI is dispensed with just by mixing red phosphorus and iodine crystals in a water solution. The red phosphorus then goes on to make HI by the above mentioned process. With a small amount of due care, this is an excellent alternative to either purchasing, stealing, or making your own pure hydroiodic acid. This method has the advantage of being easy to do. It was formerly the most popular method of making meth from ephedrine. Now red phosphorus is on the California list of less restricted chemicals, so an increased level of subterfuge is called for to obtain significant amounts. One might think that this is easily gotten around by making your own red phosphorus, but this is a process I would not want to undertake. Ever hear of phosphorus shells? I would much rather face the danger of exploding champagne bottles. Those who insist on finding out for themselves, will see Journal of the American Chemical Society, volume 68, page 2305. As I recall, the Poor Man's James Bond also has a formula for making red phosphorus. Those with a knack for scrounging from industrial sources will profit from knowing that red phosphorus is used in large quantities in the fireworks and matchmaking industries. The striking pad on books of matches is about 50% red phosphorus. The determined experimenter could obtain a pile of red phosphorus by scraping off the striking pads of matchbooks with a sharp knife. A typical composition of the striking pad is about 40% red phosphorus, along with about 30% antimony sulfide, and lesser amounts of glue, iron oxide, MnO2, and glass powder. I don't think these contaminants will seriously interfere with the reaction. Naturally, it is a tedious process to get large amounts of red phosphorus by scraping the striking pads off matchbooks. Another problem with this method is that it can produce a pretty crude product if some simple precautions are not followed. From checking out typical samples of street meth, it seems basic precautions are routinely ignored. I believe that the by-products in the garbage meth are iodoephedrine, and the previously mentioned azirine. If a careful fractional distillation is done, these products can be removed. They can be avoided in the first place if, when making hydroiodic acid from iodine and red phosphorus, the acid is prepared first, and allowed to come to complete reaction for 20 minutes before adding the ephedrine to it. This will be a hassle for some, because the obvious procedure to follow is to use the water extract of the ephedrine pills to make the HI in. The way around the roadblock here is to just boil off some more of the water from the ephedrine pill extract, and make the acid mixture in fresh pure water. Since the production of HI from iodine and red phosphorus gives off a good deal of heat, it is wise to chill the mixture in ice, and slowly add the iodine crystals to the red phosphorus-water mixture. 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. Lithium-Ammonia Reduction A three-neck flask was cooled in a dry ice/acetone bath. A condenser was fitted in the center neck, an additional funnel containing l-ephedrine base in THF was fitted into one side neck, and a rubber stopper fitted with a glass tube extending to the bottom of the flask was fitted in the third neck. Anhydrous ammonia gas was condensed and collected in the flask. Small pieces of lithium metal were rinsed in petroleum ether, patted dry, and added to the condensed ammonia. A deep royal blue color was noted as the lithium metal dissolved in the condensed ammonia. The l-ephedrine was added drop wise to the lithium ammonia solution over a period of approximately 10 minutes with stirring. When all of the l-ephedrine had been added, ammonium chloride was added slowly to the solution. The flask was removed from the cooling bath, and the condensed ammonia was allowed to warm to room temperature and evaporate from the flask through the side necks. When most of the ammonia had evaporated, water was added to the remaining solution until it cleared and any remaining lithium metal was decomposed. The remaining solution was removed from the flask to a separatory funnel, where the aqueous layer was discarded. The THF layer was dried with magnesium sulfate, and the hydrochloride salt of the methamphetamine was made by bubbling hydrogen chloride through the THF. The same procedure was used, substituting phenylproponolamine and methylephedrine as the starting materials. A second synthesis was conducted with l-ephedrine, using the same procedure except that the reaction was not quenched with ammonium chloride. It was also found that the ephedrine would reduce to methamphetamine without the addition of ammonium chloride as a quenching agent. From: eleusis@netcom.com (Eleusis) From: dmurphy3@aol.com (DMurphy3) Apparently they were following the guys handwritten notes. It would have been even more interesting had they used the real Birch method, using Na, especially when they tried the water quench. From: eleusis@netcom.com (Eleusis) I bet you they *did* do that the first time, and then, after they replaced that wing of the lab, they decided not to publish those results. From Phenylalanine Phenylalanine is 2-amino-3-phenylpropanoic acid, which is more or less amphetamine with a COOH where the CH3 should be at the end of the chain. Thionyl chloride will replace the OH with a Cl, which falls off and is replaced by H when you give it lithium aluminum hydride, sodium borohydride, or hydrogen gas and nickel/platinum. If you use hydrogen and metal for that step, you'll ha v e to reduce the carbonyl group with one of the hydrides, so best save time + effort and use them and do both reductions at once. When that carbonyl is reduced, you now have amphetamine. Go back up to that first one I mentioned for upgrading amphetamine into methamphetamine. The difference between amphetamine and methamphetamine is the addition of a single methyl group (CH3) to the amino group sticking off the middle carbon atom in the chain. Fortunately, substituting amines is really simple. Vaporize your amine (your amphetamine) with a bunch of vaporized chloromethane (CH3Cl, a solvent) and some gaseous pyridine... voila, the amino group takes the methyl from the chloromethane and lets a hydrogen go. The hydrogen joins the liberated chlorine, and the resulting HCl is soaked up by the pyridine. The pyridine is optional. Adding it drives the reaction a bit by pulling the excess HCl out of the equation, but it's not necessary. This last question is solved be reference to a principle called the law of mass action. An excess of methylamine will inhibit the secondary reactions. Typically, a reductive amination done in a parr bomb or using sodium cyanoborohydride is done with a five times molar excess of methylamine (or methylamine hydrochloride.) Make sure to use an EXCESS of acetone, because 1 its more readily available and 2 it will prevent any diphenyl/triphenyl/xphenyl acetone from forming. Hell, if your making straight amphetamine, you could even just go with acetone as the solvent too, if you could come up with a good way to separate the 2-aminopropane you'd make with the amphetamine. Given that this gunk has a bp of 33 or 34 degrees at standard pressure, it shouldn't be too hard. Smells like ammonia though... maybe you should catch it in HCl water when you distill. As with any distillation there will be some left over. Never fear, 2aminopropane (or isopropylamine) is water MISCIBLE. Yes, the BASE form is miscible w/ H2O! Amphetamine BASE is only slightly soluble in water, so if your really a purist you can dissolve your mostly amphetamine some 2aminopropane in ether and backwash with water maybe ONCE. Then precipitate the crystals with dry HCl or H2SO4? Question is, how much ammonia and reducing agent are you willing to waste on making 2aminopropane? Purification by Crystallization I wouldn't suggest ethanol or acetone as they tend to easily collect H2O; this can happen unexpectedly and when it does, their solvency power will greatly increase, redissolving your crystals. Be careful as methanol is toxic; don't get it on you or breathe the fumes. Read a lab handbook about two-solvent purification by crystallization. Fascinating stuff. Related Chemistry ---deadlock@paranoia.com Books Advanced Techniques of Clandestine Psychedelic & Amphetamine ManufactureCovers a variety of topics in the field of clandestine chemistry. Making amphetamines, MDMA (ecstasy), and other similar chemicals is what you will learn. If you have a good grasp of chemistry and know your way around a chemistry lab, you could be producing your own medicine in no time. Includes lessons on obtaining the chemicals needed to produce your chosen chemical, hydrogenation methods using electrically generated hydrogen, phenylacetone syntheses, methylamine synthesis, making bromosafrole or related substances, and more. Advanced Techniques of Clandestine...Secrets of Methamphetamine Manufacture: |
