When I started this quest, I couldn't spell Quallode and didn't have a clue what ph neutral meant.

Pass this around, spread the word.

Cheapskate
Member posted 01-20-99 02:03 PM          
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Part 1 of two parts

It will now be impossible for the DEA to prevent the synthesis of methaqualone by controlling key ingredients. The work here represents creating this schedule 1 downer that previous generations knew and loved from the most common ingredients. It's written for the beginning clandestine chemist and uses the simplest procedures and is provided for educational purposes only. This document should never be used to create illegal substances.

The basic path is starting with toluene, a common lacquer thinner, and making nitrotoluene, a precursor to TNT. Taking the nitrotoluene and making o-toluidine, a reagent used sometimes in dye making. Part of the o-toluidine is saved and the rest is used to make n-acetyl-o-toluidine, I have no idea how this reagent is used. The n-acetyl-o-toluidine is turned into n-acetyl-anthranilic acid, which seemingly has uses only in clandestine chemistry and is controlled. The n-acetyl-anthranilic acid is combined with the o-toluidine saved above to make methaqualone. This is a long path that takes time, but each step can be avoided by just getting the chemical that that step represents and moving on.

The beauty is that there is a path practically from Earth, Wind, Fire and Water to Quaalude.

The chemicals you have to buy:

Sulfuric Acid - available from hardware stores as drain cleaner.

Nitric Acid - this hasn't been found from normal sources, contact a chemical or photographic company. This isn't watched or controlled in any fashion.

Toluene - lacquer thinner. Available from hardware stores in most states. If it is controlled in your state like it is in California, get it from a fireworks supplier or some other state.

Distilled water - any grocery store. Or, if you're not very smart, it can be distilled from tap water.

Iron filings - available from fireworks suppliers. You want the 100-mesh variety.

Hydrochloric Acid - available from hardware stores as driveway cleaner or swimming pool additive.

Sodium Hydroxide - available from hardware stores as drain cleaner. Isn't it amazing how much good stuff is poured down the drain?

Glacial acetic acid - available from photography suppliers. This can also be distilled from common vinegar.

Acetic Anhydride (optional, see below) - this is watched and, in most states, controlled. It can be obtained only from chemical suppliers. There is a way around it however, see the text for explanation.

Potassium Permanganate - available from fireworks suppliers as an oxidizer.

Acetone - available from hardware stores as paint thinner.

Methanol (maybe) - available from car parts houses as fuel line defroster. A common brand name is, "Heet".

Denatured Alcohol - available from hardware stores as paint thinner. Ever notice how good stuff keeps showing up as paint thinner?

The details:

Making nitrotoluene:

This is dangerous. If the reaction gets out of control, there is a good possibility of explosion. So follow instructions and keep the temperature down.

Take 294 grams of sulfuric acid and 147 grams of nitric acid and combine them in a magnetically stirred 500 ml flask suspended in an ice water bath. The ice water bath needs to have at least 2 inches clearance on all sides from the flask and should have an inch or so clearance from the bottom of the flask. Have a lot of ice in the bath, but not so much that you can't move it around if necessary. Get the stirring going and keep a good vortex throughout the reaction. Put a thermometer in the flask and note the temperature, it should be around 18C before you start. Now measure 100g of toluene into a beaker and pour 5ml of it into the stirring acid solution. You'll see the toluene turn brown as it reacts, this brown liquid will splash on the sides of the flask leaving them brown. Note the temperature, it may rise, but usually at this point in the reaction you won't notice a change. Wait for the brown to turn yellow, this will take from a minute to several minutes depending on how much toluene you actually added, but it will happen eventually. Now add another 5 ml toluene and wait for it to turn yellow.

Continue this until you have added all the toluene. At points in the reaction you'll see the temperature rise, NEVER LET IT RISE ABOVE 60C. If it starts getting too hot, throw an ice cube in the acids. If it doesn't start to cool throw another one in. If this doesn't work, get the hell out of there. If it doesn't explode, you can continue the reaction. It is best to let the brown turn yellow and the temperature drop to 20C before adding any more toluene.

After the addition of all the toluene, let the solution set with continued stirring for 4-5 hours until the ice has melted and the water bath returned to room temperature. Now separate the acid layer from the nitrotoluene layer. The nitrotoluene layer will be the top one. The acid layer will be yellow and the nitrotoluene layer will be a much lighter yellow. If you had to add water to the mix, it will hydrate both layers and the difference in color will not be easy to see. Get a flashlight and look closely for the separation. Keep the nitrotoluene layer and pour the acid layer in your neighbors dog water bowl, we don't want to improperly dispose of toxic materials.

In a suitable size flask (probably around 500ml), add twice the volume of the nitrotoluene of water and about a teaspoon of NaOH to the raw nitrotoluene. Stir this until the NaOH has dissolved. The water layer will be orange and the nitrotoluene layer will have turned a bright yellow. Separate these and keep the nitrotoluene. Using the same flask as before (rinse it out first) add twice the volume of water (no NaOH this time), stir, and separate. This should be done until the water doesn't turn orange. The water will continue to have a slight yellow tint, this is fine. This process will yield around 150ml of bright yellow nitrotoluene. This is not getting out more than you put in even though the apparent yield is greater than 100%. There's still water in there and most of the nitrotoluene is in a form that can't be used in methaqualone synthesis. Nitrotoluene comes in three types ortho, para and meta. The difference is not necessary to understand, but the one needed is the ortho variety, which makes up about 45% of the combined total. We won't worry about separating the types at this point, since the others will fall out of the reactions to follow. This stuff smells bad and the smell will be in your clothes when you stop.

Possible screwups:

Don't screw this one up, recovery from it may require time in the hospital.

Making o-toluidine:

This is a mess and is hard to clean up. The reaction stinks of HCL and nitrotoluene and can produce fumes that can be overpowering. If you value your lungs, ventilate the hell out of the room or use a fume hood. The hot acids involved can burn clothing (skin will heal, but clothes you have to go buy). Wear safety glasses, since one splash could blind you.

In a 1 liter 2 neck distillation flask fit an overhead stirring device in the center hole. Pour 60cc of water, 120 grams of powered iron and the 150 or so ml of nitrotoluene made previously into the flask and start stirring. The stirring must be vigorous. The solutions should splash around and totally mix the ingredients. One clandestine chemist used a dremel tool with a glass rod flattened on the end attached to stir the solution. The stirring must be continued throughout the reaction. Now measure 20 ml of HCl into a cylinder. Add 10 ml of the HCl to the flask and wait for about 15 minutes. Check the temperature of the flask. Don't put a thermometer in there! You might hit the stir bar and break it dumping mercury into the reaction mix. This will not only spoil the reaction; it may create some nasty toxic substances. Just carefully feel the flask, if you can hold the flask firmly and not get burned, add another 5ml. Wait about 30 minutes (the temperature will continue to climb as the reaction progresses), check the temperature and when cool enough, add the last 5ml of HCl. Now continue the reaction until the reacting solution has returned to room temperature. This will take a couple of hours.

The only way to get the newly created o-toluidine out of the flask is by steam distillation. You can try separations, neutralization, etc. They won't work. Believe me, lots of attempts to do this have been tried, but none of them work. So set up for distillation. The best way found so far to do this is to fit the distillation adapter and condenser to the center hole (yes, get the stirring apparatus out of the way first) and use a 1 liter flask as the receiver. In the other hole of the flask put a bent glass rod that ends near the bottom of the flask through a thermometer adapter. You'll have to judge the distance by feel, the solution has turned deep black and the flask is completely coated with iron chloride. Set up a 2 liter Erlenmeyer flask to boil water in. Put a one hole stopper in the top with a glass rod in it to deliver steam. Connect the water flask and the glass tube on the two neck flask and apply heat to the water. As the water boils it will force steam into the 1 liter distilling flask and carry the o-toluidine into the condenser.

Watch the receiving flask. You'll see the water come over with some yellow stuff. As the water drips into the receiving flask you'll begin to notice a redish brown blob starting to grow, this is the o-toluidine. Continue this steam distillation until no more of the yellow stuff comes over. The receiving flask will contain around 700 ml of yellow stained water and blobs of redish brown o-toluidine. Separate the water and discard. This is not as easy as it sounds, the o-toluidine will mostly settle to the bottom, but some of it will insist on floating on top of the water. What you can do is get the stuff from the bottom, drain the water into a separate container then get the stuff from the top. Don't worry about getting all the water out, the next step will take care of that. Just concentrate on getting all the o-toluidine.

In a suitable size flask (250 ml will do it here) put the o-toluidine with three times the volume of water and about a teaspoon full of NaOH (you don't have to be careful about measuring the NaOH, as long as it all dissolves). Boil this solution briefly with stirring. Remove the solution from heat and stirring and observe. The o-toluidine will rise to the top of the solution and will be easy to separate. Pour the solution through a filter into the separatory funnel to remove any solids and separate the basic water and discard.

The yield here will be around 30ml. Disappointing isn't it. Remember that most of the yellow nitrotoluene created above was of the wrong type and didn't make it through the reaction and separation, plus there is a loss of about 35 percent even if you start with reagent grade ortho-mono-nitrotoluene (this has been tested several times).

Clean up is a bitch. The flask should be soaked in HCl to dissolve the iron mess that is now coating it. It's easiest to just fill the flask with HCl plug the necks with corks and let it set for a day or two. Then rinse and wash down as necessary.

You should do this procedure twice saving the second run for reacting later in the end stages.

Possible screw ups:

You added the entire 20 ml of HCl at once and the solution started to boil uncontrollably. It shot out of the flask and formed a volcano of hot boiling acid and iron powder. It stinks, burns and starts to destroy everything around it. Your only solution is to clean up the mess, air out the room for days and start over from scratch with new clothes. You could also move.

Making N-acetyl-ortho-toluidine:

Using Acetic Anhydride:

You don't need much of a reflux column; you can use a 400mm condenser
attached to a 500ml round bottomed flask. Put in 50ml of o-toluidine and add 50ml of acetic anhydride through the condenser, there will be an
immediate reaction and the solution will begin to boil. The fluids only
condense up about 2cm into the condenser so the one I suggested is overkill. Using a small flame, continue the boil for about 8 or 9 minutes and then dump the contents directly into a 1 liter flask filled to 900ml with room temperature dH2O. Pink crystals will immediately form. Cool the solution in the freezer until cold, but don't freeze and then filter the crystals with suction and save the mother liquid. Using gentle heat from a lamp dry the crystals and recrystalize by using just enough boiling hot alcohol to dissolve them and cooling the alcohol in a freezer for 15-20 minutes. Vacuum filter the recrystalized product from the solution and save the solution in the same flask as the first filtration thereby saving all the liquid.

After about an hour the mother liquid will have formed crystals also.
Filter this and combine with the first product, you should probably
wait a couple of hours to make sure it has all crystalized. Yield was
43 grams of white needle like crystals.

Using Glacial Acetic Acid:

The above is the easiest of the methods to date, but suppose you can't get acetic anhydride? This stuff is carefully watched and many suppliers want your life history before selling it to you. If this is the case, get glacial acetic acid. This can be ordered from photography stores, purchased (uncontrolled, unwatched) from chemical suppliers, or distilled from vinegar. Yep, this is just concentrated vinegar! Follow the above instructions, but use 100ml of glacial acetic instead of the acetic anhydride and reflux for three hours; your results will be the same. The glacial acetic will not boil on addition, just warm up a little. Oh, another advantage of glacial acetic acid is, this stuff costs around US$12.00 a gallon. This is a cheaper method by far.

Possible screwups:

You added the acetic anhydride too fast and it bubbled back up the condenser and burned your hand. Run cold water over your hand count your blessings that it didn't get your eyes and continue with whatever reagents you have left.

You left it too long in the freezer and the expanding ice broke the flask and you have icicles all over the place. Gather as much of it together as you can, thaw and proceed. You can blame the low yield on "non reagent grade chemicals."

People have reported that they couldn't get all the pink color out of the crystals, if this happens, just continue on to making n-acetyl-anthranilic acid and don't worry about it.

Making N-acetyl-anthranilic acid

This is a messy reaction. You should wear old clothes and have latex gloves handy to keep from staining your hands. Don't rub your nose while doing this, you'll look like Rudolf on a three day binge. Use 1300ml of water and dissolve 20 grams of N-acetyl-o-toluidine and 50 grams of magnesium sulfate in it with stirring while raising the temperature to 80C. This will take a few minutes; the N-acetyl-o-toluidine is hard to dissolve and should finally disappear at the 80C point. Add 50 grams of potassium permanganate which will make the solution thicker and increase the stirring speed to keep the solution from settling. You can use overhead stirring, a dremmel tool holding a glass rod flattened to a paddle at the bottom will work. If you're lucky or rich enough to have a magnetic stirring setup, cover the flask with aluminum foil to minimize evaporation. The entire mixture will work in a large Visions saucepan.

For the next three hours keep the solution at 85-90C with stirring, adding water as it evaporates. This procedure must be ventilated out a window or something so the permanganate laden steam doesn't condense on the curtains and make everything pink. At the end of 3 hours neutralize the permanganate with 30ml of denatured alcohol. The solution should turn brown and all the pink fluid should disappear. If there is some pink fluid still swirling around add another 10ml alcohol. The objective is to neutralize the permanganate. Now filter the solution hot with suction. Press a piece of plastic on top of the filter cake to get as much of the solution as possible. Add 10% sulfuric acid a few milliliters at a time to the solution with stirring and the N-acetyl-anthranilic acid will precipitate out. Filter and clean by dissolving in weak NaOH and reprecipitate by adding sulfuric as before. This should yield 16 grams of pure white crystals. If they're not pure white, see screwups below.

Possible screwups:

If you got carried away and added too much alcohol and now you can't get the crystals to precipitate out. If you add too much alcohol it will dissolve the anthranilic acid and you won't get any precipitate. If this happens, put the solution on to boil and boil away the alcohol by watching the temperature and stopping the boil when the boiling point reaches 92-95C. Let it cool and you should see the crystals forming. If not, chill it in the refrigerator. If this still doesn't work add concentrated sulfuric a couple of drops at a time until ph 2 and wait for the crystals. If they still haven't come after 8 hours, give up and start over.

You used Epsom salts instead of anhydrous magnesium sulfate and adding 50ml of 10% sulfuric still hasn't formed crystals. You should have increased the amount since the water bound up in the salt increases its weight. Also, it will take more sulfuric acid to cause the precipitation. In this case add concentrated sulfuric a drop or two at a time with stirring until precipitation occurs.

There has been at least one incident of the magnesium sulfate causing problems. To test the magnesium sulfate: put a few milliliters of water in a test tube and dissolve a gram or so of permanganate in it. The water should turn a deep purple. Add a gram or two of the magnesium sulfate to the water and stir. The magnesium sulfate should dissolve and the solution should remain purple, if you get brown precipitate and the water starts to clear, go find another source for magnesium sulfate.

When you dumped the permanganate into the hot solution it immediately boiled over and hot purple water cascaded all over the kitchen rug. The increased density of the solution and the crystals being added can cause foaming and your hard work will boil all over the counter. Remove the heat and save what you can. Bisulfide or concentrated HCL will remove most of the stains. Throw away the rug (in your neighbor's trash) and blame it on the dog.

You forgot to add the alcohol to neutralize the KmnO4 and now your filtered solution is brown to purple. Or maybe you didn't notice until after you had precipitated out the crystals and instead of pretty white, they look like mud. This is easy to fix, after drying the crystals, put them in a flask and cover with 2 to 3 times the volume of denatured alcohol. Now bring to a gentle boil with stirring for about 4 minutes. The contaminants will separate, neutralize and rise to the top; filter and dry contaminants and all. Now put the crystals and contaminants in a beaker, dissolve with dilute NaOH. You'll notice that the contaminants don't dissolve. Filter this solution at least twice, more if needed to get the contaminants out. Then, when the solution is clean, recrystalize with sulfuric as above. This will give you perfectly clean pure white crystals for the next step.

Making Methaqualone

Method 1.

Put 10 grams of N-acetyl anthranilic acid in a large test tube and add 10 grams of o-toluidine. There probably isn't enough o-toluidine to get all the anthranilic wet, so add 4 ml more and suspend the test tube in a small visions sauce pan filled with cooking oil over a hotplate. Slowly raise the temperature to about 150C. Don't make the mistake of trying to mix or compress or in any way mess around with the chemicals in the test tube. If you do, the anthranilic crystals will glue themselves to whatever you have touched them with and it will be hell trying to get them back into the solution. As the o-toluidine heats up, it will dissolve the anthranilic and condense on the side of the tube about half way up. The spreading o-toluidine will eventually dissolve all the anthranilic and start to turn dark. This is a good thing. Many folks think that the reaction has messed up at this point, it hasn't. If some of the anthranilic has escaped being captured by the o-toluidine, simply tilt and swirl the test tube until all of it is dissolved. Continue raising the temperature over the next 30 minutes until you reach 190C and keep it there. You will see bubbles being formed and rising to the top of the hot solution, this is water being evolved from the reaction, not the o-toluidine boiling. Hold it at this temperature for at least 3 hours, it can be held for a lot longer if needed (say you need to sleep or something). The solution will become dark purple and upon cooling will
be a very viscous resin.

After the 3 hours has elapsed allow the solution to cool to about 80C and pour it into 150 ml of dH2O the dark purple resin created in the previous step will settle to the bottom and stick all over the sides of the flask. You will have a mess! This is all good. Add NaOH solution to the mess until the ph reaches around 9 swirling to make sure it mixes well, the resin will solidify. Let the solution sit for an hour to assure that all the resin has solidified. Use a mixing stick to get the resin loose from the sides and bottom of the flask and swirl around to be sure it is all loose from the sides. Vacuum filter and save the (now solid) purple resin. Dry the resin and put in a suitable size flask,
you'll need about three times the volume of the solid resin.

The resin is methaqualone and nasty-purple-stuff. Dissolve the resin in about twice the volume of acetone, the acetone may have to be heated to dissolve it all. Allow the solution to cool until just above room temperature and add 10ml 34% HCL. Wait about 30 minutes. Methaqualone HCL will precipitate from the solution and settle to the bottom. Filter the solid and dry under gentle heat. You should have light purple crystals.

Alternately:

There is no need to go through a solidification process to get the methaqualone HCL, unless you need to store the stuff as a solid for some reason. Instead, after the 3 hour reaction, leave the dark purple solution in the reaction vessel (for this you should probably use a 250ml flask of some sort) and add twice the volume of acetone. Stir the acetone until all the purple stuff has dissolved and then add the same volume of 34% HCl as purple stuff. Be careful, if the acetone is hot, addition of the HCl will cause it to boil. Now bring the entire solution to a gentle boil for about 4 minutes, remove the heat and allow it to cool. After being cool for about 1.5 hours crystals will form, eventually becoming a slurry of crystals in purple stuff. If you're in a hurry, refrigerate. If there are no crystals, get a couple of drops of the chilled fluid on a stir stick and dry them with gentle heat (a flame-thrower is NOT appropriate). Drying will form sticky goo with a few crystals in it, return the stir stick to the flask and swirl to get the crystals into the solution. The purple fluid will start to crystallize in a hurry. Filter the crystals dry and proceed to purification.

Purification:

Now begins the purification process. Put the crystals in a beaker and add roughly twice the volume of acetone, toss in a few boiling granules and gently boil the acetone. Boiling granules are small chips of chemically inert material that have a very porous surface. They help the boil start faster and stay under control. If you don't have these, go break one of your neighbor's windows and collect some glass pieces around 3mm in size. The crystals will not dissolve, but the left over nasty-purple-stuff will. Filter the crystals and dry. If, after drying, there is a purple tint to the crystals, then recrystalize from methanol. To do this, put the crystals in a small beaker add just enough MeOH to get them wet and start heating the mix. Some of the crystals will dissolve immediately, if they don't all dissolve bring the MeOH to a boil and add MeOH a little at a time, maintaining boiling until they have all dissolved. Now continue the boil until about 20% of the MeOH has been evaporated. Allow the solution to cool and wait. After about an hour there will be crystals forming and clinging to the sides of the tube, wait until you're sure all the crystals have formed and filter. Use acetone to wash the crystals out of your flask and to rinse as much of the nasty-purple-stuff from the crystals in your filter paper. Save both the solution and the crystals.

The recrystalization will help some, but will not purify the crystals. What has happened is that during the reaction, the nasty-purple-stuff has wrapped itself around and within the crystalline structure of the methaqualone and recrystalization will create a new surface so a acetone wash will be able to get the rest. Now repeat the acetone boil described above and filter and dry. You should have light steel grey to white powder, if you do, stop and put this batch aside, if you don't, do another acetone wash.

Remember the solution you saved from the recrystalization above? This is nasty-purple-stuff, MeOH, acetone and methaqualone. Put a few boiling granules in the solution and boil away half the volume. Let this set and cool and more methaqualone will precipitate out. This can be purified with acetone as above and the result added to your completed batch. You can repeat this process until almost all the methaqualone has been recovered from the solution, but each recovery will be less pure. If you choose to do this, combine all the recovered product and do one last acetone boil to clean it up.

Possible screwups:

Ok, you couldn't wait and you tried to stir the o-toluidine and n-acetyl-anthranilic acid mix. The sides of the tube are covered with sticky crap and the stir stick has goo all over it too. You can't get the stuff loose without it sticking to everything and you have a blister on your finger where you touched it to see if it was still hot. The best you can do now is to just put the stir stick in the tube and go find something to do somewhere else for the next 45 minutes. The solution will react and the temperature will go up. Eventually the solution will turn purple and the stuff on the sides of the tube and stir stick will melt down into the solution. You won't get 100% recovery, but remember, I told you not to mess with it.

You took too long letting the purple liquid cool and now its so viscous it won't pour out of the tube into the water. Just heat it gently while holding it upside down over the water. Don't hold it with your hands or you'll have another blister to match the one on your finger from above.

You poured the purple viscous liquid into the 150ml of water and took the ph to 9 stirring all the time to make sure it mixed well, but a big glob of the sticky purple stuff has adhered to the stir stick and you can't get it loose. Don't worry, just leave it in the flask and let the stuff solidify. After solidification it's easy to get it off.

The purple viscous liquid has been in the water at ph 9 for 4 hours now and it still isn't solid. OK, raise the ph to 11 and mix the solution a lot. If you can, shake it real good (an Erlenmeyer flask is good for this). This should cause solidification. If it still doesn't solidify, pour off the water as much as possible and dissolve in acetone as above then add concentrated HCL to form the hydrochloride. Now just go through the purification process.

When drying the solidified purple stuff, you used a light to warm it gently and accelerate the process. Unfortunately, the 300 watt halogen light you used melted the purple resin. The melted resin soaked into the filter paper and stuck to the plate you had under it. Well, at least the water dried out. Take the paper shove it into a flask then wash the plate with methanol catching the solvent in the same flask. Now gently heat the flask, paper methanol and all. When the purple solid has dissolved from the paper (you'll never get it all) remove the paper, wring it out and throw it away. Now filter the methanol while hot and begin boiling the methanol to reduce its volume. After reducing to about 1/2 the volume let it cool and add dH2O until it clouds up. Add NaOH until the ph reaches 9 and the purple solid will separate from solution. Filter the solid and dry again. This time, don't melt it.

You didn't use boiling granules to control the boiling acetone wash and the acetone "bumped," erupting hot solvent all over the place. Remove the flask from the heat, turn off the heat and let everything (including your temper) cool down. Now go get a hammer and break the neighbor's window as instructed above and resume with whatever amount you have left. This time though, use the damn boiling granules.

Method 2.

This is essentially the same as above, but uses polyphosphoric acid to bind the water instead of just evaporating it. Put 20 grams of polyphosphoric acid in a rb flask and begin warming it. This is not as easy as it sounds. Polyphosphoric acid is very viscous and hard to pour. If you warm it to help the pouring some, you have to get it so hot it's hard to handle. I suggest you place a test tube in an Erlenmeyer flask put them both on the scale and pour the acid directly into the test tube until you get about 18 grams in the tube. Stop pouring, by the time you've pulled the syrupy fluid back without getting it all over everything, you'll have about 22 grams in the tube. Now take the tube out and invert it over the rb flask and gently heat it with a torch to help the acid flow down into the flask. Just leave the tube in the flask while you measure the other items. Add however much of the N-acetyl-anthranilic acid you have (up to 10 grams) and an equimolar amount of o-toluidine. raise the temperature slowly to about 160C and, using a stir stick, stir the solution. Yes, it's ok to stir this reaction. It actually helps the solid dissolve. Your stir stick will accumulate a sticky resin, but just leave it in the flask and it will take care of itself. After the solid has dissolved, raise the temperature to 180-190C for 20 minutes.

Allow the solution to cool to less than 100C, it will be yellow or orange, and pour into 150ml of dH2O. Stir the solution in the water until it dissolves. It really will dissolve, it is sticky and will cling to everything, but it will eventually dissolve. Now take the water solution and pour it into the rb flask you did the reaction in and swirl around until you dissolve the part you couldn't pour out of the rb flask. Put the solution into a larger flask, 500ml or better and add soda lime solution until neutral. This will take a lot to neutralize and will result in a yellow or orange resin that sticks to the side of the flask like the above reaction. It will solidify after setting for a couple of hours. Filter and dry the solid then follow the purification as above. Since the o-toluidine hasn't been hot as long and the water has been isolated by the polyphosphoric acid there is minimal charring and minimal cleanup. You are likely to get white crystals.

Possible screwups:

You used too much polyphosphoric acid and had to add a ton of soda lime to neutralize it. Now you're stuck with some salt or other in the solution with your yellow resin. Filter all the solids out and dump them into about 200ml of dH2O and heat. The solids will dissolve and the resin will melt collecting in a puddle at the bottom of the water. Let this cool until the resin solidifies then filter. You'll have only the resin left, now proceed with the purification.

You used a propane torch to boil the acetone during the wash. The acetone boiled over and caught fire from the torch. You tried to pat out the fire, but only managed to set your shirt on fire also. Now the fire department is pulling up in the driveway with a police escort. Well, I suggest you wrap a towel around the burned arm and put another around the blistered hand and run!

Method 3:

This was done by a different chemist than the above, so not as many mistakes were made. The voice for this is The Alchemist.

Ok, here it goes....

Methaqualone from Anthranilic Acid
----------------------------------

The following, of course, is for educational purposes only...

10g of anthranilic acid was dissolved in 30mL of acetic anhydride in a 100mL RB flask, at which point the flask became very hot and the reaction was apparent as small amounts of the anthranillic dissolved and acetic anhydride became a pinkish tint. To this was added a stirbar (better do this before you add chemicals or stirring will become difficult) and a distillation setup was attached without vacuum. The flask was set spinning and the temp raised progressively to 190°C.

Around 160°C the acetic anhydride and acetic acid began to distill over. Do this until almost all the acetic anhydride has distilled over. Turn off the heat and wait until the temp reaches 70°C. When the flask cools off, you may get some wet solid looking material in the flask (N-acetylanthranilic acid). It gets pretty hard so you might want to break it up with a spatula or something so it can stir. Once the temp has reached around 70°C, add 10g of o-toluidine(9.9mL). Replace the distillation setup and raise the temp once again to 190°C. Hold it there for three hours. The appearance of water coming over the distillation setup will be apparent during the first half of the reaction. Turn off heat. When temp reaches 80°-90°C, dump resin into 150mL of distilled H20. Basify the soln. from 9-12. Stick it in the freezer to make it more solid. When it sits in the freezer for about 20 min, take it out, dump off the water and wash it with a little distilled water. This shit should be stuck all over the bottom of your flask or beaker. Add 150mL of acetone and swirl until dissolved. Sometimes this takes a while so you may want to heat the acetone. Once it has all dissolved you will have a purplish-amber soln with no solid in the flask. Once it is all dissolved, add 10mL conc. HCl. Crystals should form upon standing for at most a half hour. If no crystals form stick soln in the freezer and force them out of solution. Filter these crystals and wash them with a little acetone. Dry the crystals and add them to a flask with 100 mL fresh acetone. Boil the acetone with the crystals in them for at least 10min. This should get your methaqualone crystals snow white. Dry your product and enjoy!

This is a very clean and easy reaction that produces 70%+ yields. Props go to Cheapskate for his easy cleanup procedure for producing extremely high grade 'ludes.

The Alchemist

Super purification:

This Cheapskate talking again. Now you've got pretty steel gray or white crystals and the celebrating has begun, but you can do better. Methaqualone.HCl will dissolve in acidic water, so mix up two flasks of water at ph 3 and add your methaqualone.HCl to one of them. Boil the methaqualone until it dissolves in the acidic water, you'll notice there is a small amount of stuff that won't dissolve. Filter the boiling hot solution into a suitable flask and rinse the filter paper through the funnel with the other flask of hot water. Allow the water to cool and chill to recover the crystalline methaqualone.HCl. This will be pure white fluffy crystals with the only contaminant left being the filter fibers that you scrap off when you gather the crop.

Cheapskate

Cheapskate
Member posted 01-20-99 02:12 PM          
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Whew....

Rhodium
Administrator posted 01-20-99 02:32 PM          
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GREAT post Cheapskate! This will be included in my FAQ asap! Now the only thing left is the conversion of napthalene (mothballs) to anthranilic acid, using only OTC reagents.

Naphtalene ==H2SO4/Hg==> Phtalic acid ==Heat==> Phtalic anhydride ==Ammonia==> Phtalamide ==Chlorox/NaOH==> Anthranilic acid

Bright Star
Member posted 01-20-99 02:48 PM          
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FAN FUCKING TASTIC. DETAIL EXTRODONAIRE!!!

Looks like I'm spending more time in the basement. DAMN! MUAHAHAHAHAHAHAHAHAHA!!!!

rexAMINE
unregistered posted 01-20-99 07:19 PM           
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Yeah great work cheapskate but nitric acid is a very suspicious chemical and very hard stuff to get rid off in a hurry. Also making nitro toluene isn't as hard and dangerous as you make it seem to be. Honest I made this in organic chemistry in high school. Just makesure the temp doesn't rise above 50C. You can be fairly careless with temperature and it will not blow up. We use the ice from the ice bath to throw at each other and let the temp reach 80C and nothing happened.

OK sorry for being kinda arrogant I know you know tons more then me.

Piglet
Member posted 01-21-99 03:59 AM          
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Amazing stuff indeed. In reply to your safety concerns over the nitro-toluene production, maybe making nitroso-toluene using nitrous acid would be an alternative? The reduction proceeds the same way, so it doesn't affect any other part of the synthetic pathway. It affords the use of NaNO2 to make the acid so it's pretty unwatched (as far as I know!!).

Fantasitc stuff,
Piglet

PS I'm hoping to improve my chemistry like you have. To that end, this week sees an intensive program to get that Clomethiazole synthesis working (PTC scavanging time!). Thanks for the inspiration 

Cheapskate
Member posted 01-21-99 10:40 AM          
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To rexAMINE: Your right, In the hundred or so times I did the nitro reaction it got out of hand and shot off for the moon temperature-wise and I never had an explosion. However, given the skill level of some of our participants I'd rather err on the side of safety, new clandestine chemists are hard to find.

Also, it's kind of fun writing it up that way. It's my FAQ, can't I have some fun too?

To Rhodium: Thank you. The mothball idea is great, there's something cool about making Quaaludes out of mothballs. I'll start looking into it....when I sober up.

To piglet: I never thought of using nitroso-toluene!! I'll have to consider this.

But isn't this cool?!? Quaaludes made from paint thinner, drain cleaners, fireworks oxidizers, metal filings and vinegar!!

I need some pigs ears....I wonder what the market is for silk purses this year.

Piglet
Member posted 01-21-99 11:03 AM          
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CS: Stop looking at my ears, man!

Dick
unregistered posted 01-22-99 10:08 PM           
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You are my Hero cheapskate here is another interesting synth. black powder can be bought at gun shops used in gun powder mixed with sulfuric acid and slowly heated and distilled will make nitric acid don't know the exact recipe . this might help some keep up the good work> 

Piglet
Member posted 01-27-99 05:51 AM          
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CS: RE: Nitrosotoluene: thess compounds are more toxic than nitrotoluene but having MPs between 45-75C, at least they arn't volatile. You iron reduction should work fine, but since you mentioned the mess, I wondered if maybe a basic Zn/Cu reduction might suit you better? (Zn + CuCl in NaOH solution. Details in Vogals).

TTFN,
Piglet 

Piglet
Member posted 01-27-99 10:47 AM          
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Also, seperation might prove fun. You might have to make the mixed toluidine & distill that to seperate. But at least you avoid nitric acid. If someone knows the % of each formed, that would help a lot...

Cheapskate
Member posted 01-27-99 07:14 PM          
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Piglet, could you post the relevant details of the Zn/Cu reduction? The nearest Vogel's is at a university that is 20+ miles away and charges $20 to park.

Piglet
Member posted 01-28-99 06:52 AM          
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CS: I will type it up for you. It's quite big, so give me a couple of days. I have a number of possibly useful reductions, could you give me an E-mail address (just set up a temporary hotmail account if you are worried about giving your real address away) and I will send you them.

Happy to help,
Piglet

PS Also, I want your opinions on the 'Hemi' synth...

Cheapskate
Member posted 01-28-99 01:20 PM          
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Cheapskate77@hotmail.com

I guess it disapeared from the profile.