The first thing he does is test the chemicals. He puts 5 ml of phenylacetone and 10 ml of N-methylformamide in a clean dry test tube or similar small glass container. Within a few seconds they should mix together entirely. At this point, he may offer a prayer to the chemical god, praising his limitless chemical power and asking that some of this power be allowed to flow through him, the god's High Priest. He may also ask to be delivered from the red tar that can be the result of this reaction. If they do not mix, there is water in the Nmethylformamide. In this case, he must distill it again, being more careful this time. Having tested the chemicals, he is ready to proceed with the batch. (However, if the underground chemist was reckless enough to obtain N-methylformamide ready made, he will have to distill it under a vacuum before it can be used in this reaction.) The phenylacetone he made (about 100 ml) is mixed with the N-methylformamide. The best amount of N-methylformamide to use is about 250 ml, but any amount from 200 to 300 ml will work fine. With 200 ml of N-methylformamide, there are about four molecules of N-methylformamide to one of phenylacetone. This is the bare minimum. With 300 ml, the ratio is nearly six to one. Any more than this is a waste of N-methylformamide. The best flask for mixing them is a 500 ml round bottom flask. After they are mixed, this flask is set up as shown in Figure 9. The flask is sitting in an oil bath, to supply even heating to the flask. The oil (once again, Wesson is a good choice) should extend about 2/3 of the way up the side of the flask. A metal bowl makes a good container for this oil bath. This is better than a pan, because it will be important to see into the flask. The fact that the oil will expand when heated is kept in mind when filling the bowl with oil. A thermometer is also needed in the oil bath to follow its temperature. The test material is added to the flask. The heat source to the flask is turned on. A low heat setting is used so that the rise in temperature can be closely controlled. The thermometer used in the distillations is placed (clean and dry) inside the flask. The rise in temperature of both the oil bath and the flask is monitored. The contents of the flask are stirred regularly with the thermometer. The temperature of the oil bath is brought to lOOQ C over the course of about 45 minutes. Once it reaches this level, the heat is turned back down a little bit to stabilize it in this area. The chemist must closely control every degree of temperature increase from here on. The temperature of the contents of the flask is worked up to 105g C. The contents of the flask are stirred every 15 minutes. At about lOSQ C, the reaction kicks in, although sometimes the heat must go as high as 110g C before it starts. When the reaction starts, the contents of the flask begin to bubble, sort of like beer, except that a head does not develop. A trick to get this reaction going at a nice low temperature is to gently scrape the thermometer along the bottom of the flask. Although I have never had the sophisticated equipment to prove it, it is a pet theory of mine that this is because ultrasonic waves are generated, producing a condition of resonance with the reactants that causes the reaction to start. The chemist wants to keep the temperature down at the same level at which the reaction first kicked in for as long as the reaction will continue at that level. Generally, it can go for a couple of hours at this level before the reaction dies down and an increase in temperature is necessary. The reaction mixture has the same color as beer and gently bubbles. The bubbles rise up from the bottom of the flask, come to the surface, and then head for where the thermometer breaks the surface. Here they collect to form bubbles about 1 centimeter in size before they break.This may look like boiling, but it is not. Everything inside the flask has a much higher boiling point than the temperatures being used. These are actually bubbles of carbon dioxide gas being formed as by-products of the reaction. The chemist can tell how well the reaction is going by the amount of bubbling going on. When the rate of bubbling slows down to almost stopping, it is time to raise the temperature. It should only be raised about 3g C. This requires turning up the heat only slightly. The highest yield of product is obtained when the lowest possible temperature is used. For the duration of the reaction, the contents of the flask are stirred with the thermometer every half hour. And so the reaction is continued. As the reaction dies down at one temperature setting, the temperature is raised a few degrees to get it going again. It will be able to stay in the 1209 to 130Q C range for a long time. The reaction has a lot of staying power in this range. Finally, after 24 to 36 hours, 140Q or 145Q C is reached. The reaction stops. The chemist takes his time working up to this temperature because the amount and quality of the product depends on it. Once 140ø to 145ø C is reached and the reaction stops, the heat is turned off and the contents allowed to cool down. It should still look like beer. A reddish tint means that his prayer failed and he was not delivered from the tar. Even so, there's still lots of good product in it. While it is cooling down, the underground chemist gets ready for the next step in the process. He is going to recover the unused methylamine for use in the next batch. This cuts his consumption of methylamine to about half of what it would be without this technique. What he is going to do is react the unused N-methylformamide with a strong solution of sodium hydroxide. The N-methylformamide is hydrolyzed to form methylamine gas and the sodium salt of formic acid (sodium formate). In chemical writing, this reaction is as follows: [SNiP] The methylamine gas produced is piped into formic acid to make N-methylformamide for use in the next batch. First, 6 ounces (about 180 grams) of sodium hydroxide pellets are added to 450 ml of water. A good quality lye is an acceptable substitute. Eye protection is worn. Once the solution has cooled down, it is poured in a 2000 ml round bottom flask with 5 boiling chips. Then all of the methamphetamine reaction mixture is poured into the flask along with it. It is swirled around a little bit to try to get some of the N-methylformamide dissolved into the water. This does not accomplish much, however, as the reaction mixture floats on the sodium hydroxide solution. The glassware is set up as shown in Figure 8 in Chapter 4. The 2000 ml flask containing the NaOH solution and the methamphetamine reaction mixture sits on the heat source. The bent piece of glass tubing once again leads to a 1000 ml round bottom flask equipped with a condenser. The 1000 ml flask once again contains 250 ml of 88% formic acid. The heat source is turned on to about 1/3 maximum. The flow of ice water through the long condenser is begun. In a while, the boiling chips float up to the interface of the sodium hydroxide solution and the reaction mixture, and some bubbling and frothing of the reaction mixture begins. The heat is turned down some, since the temperature of the mixture should rise slowly from now on. That is because the hydrolysis reaction forming methylamine tends to kick in all at once, if this precaution is not taken, leaving the chemist in a dangerous situation with a runaway reaction. After the first rush of the reaction has subsided and the bubbling of the methylamine into the formic acid has slowed down, the heat applied to the 2000 ml flask is increased to maintain a good rate of methylamine flow to the formic acid. Eventually, all the methylamine will be boiled out. This will be when methylamine no longer flows evenly into the formic acid. The flask must not be heated so strongly that water is forced through the bent glass tubing. The heat is turned off and the level of the flask containing formic acid is lowered so that the acid is not sucked back into the other flask. This formic acid is about half reacted with methylamine. When it has cooled down, it is poured in a tall glass bottle and kept in the freezer until the next batch is made, when it is used for the production of Nmethylformamide. Since it is already half reacted, the amount of methylamine used is reduced accordingly. Meanwhile, back in the 2000 ml flask, the methamphetamine reaction mixture is about 100 ml in volume and has a red color. It floats above the sodium hydroxide solution. Once it has cooled down, the contents of this flask are poured into a 1000 ml sep funnel. The sodium hydroxide solution is drained out and thrown away. The red methamphetamine formyl amide is poured into a 500 ml round bottom flask with 3 boiling chips. 200 ml of hydrochloric acid is measured out. (The 28% hardware store variety is fine for this purpose.) It is poured into the sep funnel and swirled around to dissolve any product left behind in the sep funnel. Then it is poured into the 500 ml flask with the product. When swirled around, they mix easily. The glassware is set up as shown in Figure 2b in Chapter 3. Tap water flow is proper for use in the condenser. The heat is turned on to the 500 ml flask, and a gentle rate of boiling is maintained for 2 hours. The mixture quickly turns black. The reaction going on here is metharnphetamine formyl amide reacting w~th hydrochloric acid to produce methamphetamine hydrochloride and formic acid. This is a hydrolysis reaction. After the two hours have passed, the heat to the flask is turned off. While the flask is cooling down, 80 grams of sodium hydroxide and 250 ml of water are mixed in a 1000 ml round bottom flask. Once again, a good quality lye is acceptable. If the 35% laboratory grade of hydrochloric acid was used in the last step, then 100 grams of sodium hydroxide is mixed with 300 ml of water. When both flasks have cooled down, the black reaction mixture is cautiously added to the sodium hydroxide solution. It is added in small portions, then swirled around to mix it. They react together quite violently. The reaction here is sodium hydroxide reacting with hydrochloric acid to produce table salt, with formic acid to produce sodium formate, and with methamphetamine hydrochloride to produce methamphetamine free base. When the sodium hydroxide solution gets very hot, the chemist stops adding the reaction mixture to it until it cools down again. After all the black reaction mixture has been added to the sodium hydroxide solution, there is a brown liquid layer floating above the sodium hydroxide solution. This brown layer is methamphetamine free base. It also has a good deal of unreacted methamphetamine hydrochloride dissolved in it. This latter has to be neutralized because it will not distill in its present form. The 1000 ml flask is stoppered and shaken vigorously for 5 minutes. This gets the methamphetamine hydrochloride into contact with the sodium hydroxide so it can react. The bottom of the flask is full of salt crystals that cannot dissolve in the water because the water is already holding all the salt it can. The chemist adds 100 ml of water to the flask and swirls it around for a few minutes. If that does not dissolve it all, he adds another 100 ml of water. After the flask has cooled down, it is poured into a 1000 ml sep funnel, and 100 ml of benzene is added. The sep funnel is stoppered and shaken for 15 seconds. It is allowed to stand for a couple of minutes, then the lower water layer is drained into a glass container. The brown methamphetamine-benzene layer is poured into a clean, dry 500 ml round bottom flask. The water layer is extracted once more with 100 ml benzene, then thrown away. The benzene layer is poured into the 500 ml flask along with the rest of the methamphetamine. The chemist is now ready to distill the methamphetamine. He adds three boiling chips to the 500 ml round bottom flask and sets up the glassware for fractional distillation as shown in Figure 5. The 500 ml flask sits directly on the heat source. The glass-packed claisen adapter is the proper fractionating column. The collecting flask is a 250 ml round bottom flask. Tap water is used in the condenser. The heat source is turned on to 1/4 to 1/3 maximum. Soon the mixture begins boiling. The first thing that distills is benzene water azeotrope at 68ø C. Then pure benzene comes over at 80øC. Once again, as in the distillation of phenylacetone, foaming can sometimes be a problem. In that case, it is dealt with in the same way as described in Chapter 3. When the temperature reaches 85øC, or the rate of benzene collecting slows to a crawl, the heat is turned off and the flask allowed to cool down. The collected benzene is poured into a bottle. It can be used again the next time this process is done. The same 250 ml flask is put on the collecting side. The distilling flask is now cool, so vacuum is applied to the glassware at full strength. The last remnants of benzene begin to boil, and the heat is turned back on to 1/3 maximum. The temperature begins to climb. If an aspirator is being used, when the temperature reaches 80-ø C, the chemist quickly removes the vacuum hose and replaces the 250 ml flask with a clean dry one. If he is using a good vacuum pump, he makes this change at about 70øC. The flask change is done quickly to avoid overheating in the distilling flask. The methamphetamine distills over. With an aspirator, the chemist collects from 80øC to about 140ø or 150ø C, depending on how strong the vacuum is. With a vacuum pump, he collects to about 120ø or 130øC. Once it has distilled, the heat is turned off and the vacuum hose disconnected. The product is about 90 ml of clear to pale yellow methamphetamine. If the chemist is feeling tired now, he may take out a drop on a glass rod and lick it off. It tastes truly awful and has a distinctive odor, somewhat biting to the nostrils. He is now ready to make his liquid methamphetamine free base into crystalline methamphetamine hydrochloride. Half of the product is put into each of two clean dry 500 ml Erlenmeyer flasks. The chemist now has a choice to make. He can use either benzene or ethyl ether as the solvent to make the crystals in. Benzene is cheaper, and less of it is needed because it evaporates more slowly during the filtering process. Ether is more expensive, and flammable. But since it evaporates more quickly, the crystals are easier to dry off. If ether is used, it is anhydrous (contains no water). A third choice is also possible for use as a crystallization solvent. This is mineral spirits available from hardware stores in the paint department. Mineral spirits are roughly equivalent to the petroleum ether or ligroin commonly seen in chem labs. Those brands which boast of low odor are the best choice. Before using this material it is best to fractionally distill it, and collect the lowest boiling point half of the product. This speeds crystal drying. Since the choice of mineral spirits eliminates ether from the supply loop, the clandestine operator may well go this route. Toluene is also an acceptable solvent. With the solvent of his choice, the chemist rinses the insides of the condenser, vacuum adapter and 250 ml flask to get out the methamphetamine clinging to the glass. This rinse is poured in with the product. Solvent is added to each of the Erlenmeyer flasks until the volume of liquid is 300 ml. They are mixed by swirling. A source of anhydrous hydrogen chloride gas is now needed. The chemist will generate his own. The glassware is set up as in Figure 10. He will have to bend another piece of glass tubing to the shape shown. It should start out about 18 inches long. One end of it should be pushed through a one-hole stopper. A 125 ml sep funnel is the best size. The stoppers and joints must be tight, since pressure must develop inside this flask to force the hydrogen chloride gas out through the tubing as it is generated. Into the 1000 ml, three-necked flask is placed 200 grams of table salt. Then 35% concentrated hydrochloric acid is added to this flask until it reaches the level shown in the figure. The hydrochloric acid must be of laboratory grade. Some concentrated sulfuric acid (99-98%) is put into the sep funnel and the spigot turned so that 1 ml of concentrated sulfuric acid flows into the flask. It dehydrates the hydrochloric acid and produces hydrogen chloride gas. This gas is then forced by pressure through the glass tubing. One of the Erlenmeyer flasks containing methamphetamine in solvent is placed so that the glass tubing extends into the methamphetamine, almost reaching the bottom of the flask. Dripping in more sulfuric acid as needed keeps the flow of gas going to the methamphetamine. If the flow of gas is not maintained, the methamphetamine may solidify inside the glass tubing, plugging it up. Within a minute of bubbling, white crystals begin to appear in the solution. More and more of them appear as the process continues. It is an awe-inspiring sight. In a few minutes, the solution becomes as thick as watery oatmeal. It is now time to filter out the crystals, which is a two-man job. The flask with the crystals in it is removed from the HC1 source and temporarily set aside. The three-necked flask is swirled a little to spread around the sulfuric acid and then the other Erlenmeyer flask is subjected to a bubbling with HC1. While this flask is being buWled, the crystals already in the other flask are filtered out. The filtering flask and Buchner funnel are set up as shown in Figure 11. The drain stem of the Buchner funnel extends all the way through the rubber stopper, because methamphetamine has a nasty tendency to dissolve rubber stoppers. This would color the product black. A piece of filter paper covers the flat bottom of the Buchner funnel. The vacuum is turned on and the hose attached to the vacuum nipple. Then the crystals are poured into the Buchner funnel. The solvent and the uncrystallized methamphetamine pass through the filter paper and the crystals stay in the Buchner funnel as a solid cake. About 15 ml of solvent is poured into the Erlenmeyer flask. The top of the flask is covered with a palm and it is shaken to suspend the crystals left clinging to the sides. This is also poured into the Buchner funnel. Finally, another 15 ml of solvent is poured over the top of the filter cake. Now the vacuum hose is disconnected and the Buchner funnel, stopper and all, is pulled from the filtering flask. All of the filtered solvent is poured back into the Erlenmeyer flask it came from. It is returned to the HC1 source for more bubbling. The Buchner funnel is put back into the top of the filtering flask. It still contains the filter cake of methamphetamine crystals. It will now be dried out a little bit. The vacuum is turned back on, the vacuum hose is attached to the filtering flask, and the top of the Buchner funnel is covered with the palm or a section of latex rubber glove. The vacuum builds and removes most of the solvent from the filter cake. This takes about 60 seconds. The filter cake can now be dumped out onto a glass or China plate (not plastic) by tipping the Buchner funnel upside-down and tapping it gently on the plate. And so, the filtering process continues, one flask being filtered while the other one is being bubbled with HC1. Solvent is added to the Erlenmeyer flask to keep their volumes at 300 ml. Eventually, after each flask has been bubbled for about seven times, no more crystal will come out and the underground chemist is finished. If ether was used as the solvent, the filter cakes on the plates will be nearly dry now. With a knife from the silverware drawer, the cakes are cut into eighths. They are allowed to dry out some more then chopped up into powder. If benzene was used, this process takes longer. Heat lamps may be used to speed up this drying, but no stronger heat source. The yield of product is about 100 grams of nearly pure product. It should be white and should not get wet, except in the most humid weather. It is suitable for any purpose. It can be cut in half and the underground chemists will still have a better product than their competition. But they will not cut it until a few days have passed, so that their options are not limited should one of the problems described in the next few paragraphs arise.
Personally i do not understand what lOOQ C means but see it written in other synthesis's or the oil bath as to what that exactly means but other than that this synth seems rather easy and is from a book. "Secrets of Methamphetamine Manufacture" There is also some other synth using lithuim batterys that can get 100g and its rather fast and easy. If anyone knows that synth on here show me link.
The hard part of that synth will be getting your hands on the P2P and methylamine. Not exactly OTC items. A 100 gram synth using AA and lithium suffers from the problem of finding that much psuedo, but the info is widely available. www.googlethatfucker.com
If you want the synth for P2P, methylamine, methylfromide, and more its in the book. I can post the synths it starts basically with getting everything over the counter to be able to make 100g's till you can upgrade for under 500 bucks inculding all glassware(not inculding vacuum).
