I quickly put this together to assist me in writing about Chuck. It has been paraphrased and shortened. All credit is due to CheapSkate. I also find this an easier format to reference if I have any questions.
Caution written by a non-chemist. Has not yet been checked for errorsThe chemicals you have to buy:
* Sulfuric Acid - 294g (additional will be needed * )
* Nitric Acid - 147g
* Toluene - 100g
* Distilled water - Gallon or two
* Iron filings - 120g
* Hydrochloric Acid - 20ml
* Sodium Hydroxide - 3 teaspoons *
* Glacial acetic acid - 100ml
* Acetic Anhydride (optional, see below) - 50ml
* Potassium Permanganate - 50g
* Acetone - approx 1 L
* Methanol - approx 1 L
* Denatured Alcohol -approx 1L
* Mag Sulfate - 50g
*Amounts are unknown. However, not much is needed.
Equipment:
* Boiling granules
* 1 L 2 Neck flask
* Separatory Funnel (1 L or larger)
* Thermometer
* Hotplate / Stirrer or overhead
* 200mm Condensor(400 reccomended by Cheapskate)
* Test Tube
* Thermometer adapter
* 2 + L flash or other large vessel(Cheapskate uses visionware)
* Latex Gloves
* Steam (Use a pressure cooker. Cheapskate uses a 2L elnmr flask)
* Tubing(Glass reccomended by Cheapskate)
* 250ml glask
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.
1) 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. Have 2 inches of clearence on all sides of(Make sure flask can move). Temperature of flask should be 18c or lower before proceeding.
2) Now measure 100g of toluene into a beaker and pour 5ml of it into the stirring acid solution. The toluene will turn brown as it reacts. Wait for the brown to turn yellow, this will take from a minute to several minutes depending on how much toluene you actually added. Now add another 5 ml
toluene and wait for it to turn yellow. Continue this until you have added all the toluene. Allow tempature to drop to 20c between toluene additions and never let the temp rise above 60c. If it does you may die.
3) After the addition of all the toluene, let the solution set with continued stirring for 4-5 hours.
4) Grab sep funnel. Seperate the nitrotoluene from the acid layer(Nitro will be a much lighter yellow).
5) Clean the 500ml flask. Add 2x the volume of the nirto of water and a teaspoon of NaOH. Stir until NaOH dissolves. Water layer will be orange and the nitro will have turned a bright yellow. Keep nitro layer.
6) Seperate both layers. Rinse 500 ml flask, again. Follow step 5 but no NaOH this time. Repeat step 5 without NaOH until water layer does not turn orang). Eventually water will just have a yellow tint.
Yield approx 150ml of bright yellow nitrotoluene.
Making o-toluidine:
1) 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 ml of nitrotoluene into the flask and start stirring. The stirring must be vigorous.
2) While stirring add 10 ml of the HCl to the flask and wait for about 15 minutes. When flask is cool enough to handle continue.
3) Add 5ml of Hcl, wait for flask to cool(30 min) then add another 5ml of hcl.
4) Allow things to cool and settle for a couple of hours.
5) Set up for steam distillation. Fit distillation adapter to center hole and use 1L flask for receiver. In other hole you will need to deliver steam. Cheapskate suggests using a bent glass rod connected to the flask by a thermometer adapter. Then connect the rod to a 2L Erlenmeyer flask(This will be source of steam)
6) Seperate water from o-toluidine.
7) Place o-toluidine with 3x volume of water and a teaspoon of NaOH in a 250ml flask
Boil 'briefly' and stir. Remove from heat & watch. O-toluidine should 'surface'.
9) Pour solution through filter to remove solids.
Yield approx 30ml of O-toluidine
Making N-acetyl-ortho-toluidine:
Using Acetic Anhydride:
step skipped(See cheapskate writeup)
1) Attach 400mm condenser to a 500ml round bottomed flask. Put in 50ml of o-toluidine and add 100ml of
glacial acetic acid through the condenser. The fluids only condense up about 2cm into the condenser. Reflux for 3 hours. **
2) Dump the contents directly into a 1 liter flask filled to 900ml with room temperature dH2O. Pink crystals will immediately form.
3) Cool the solution in the freezer until cold, but don't freeze.
4) Filter the crystals with suction and save the mother liquid.
5) Using gentle heat from a lamp dry the crystals and recrystalize by using just enough boiling hot alcohol
to dissolve them. Now cool the alcohol in a freezer for 15-20 minutes.
6) 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.
7) After about an hour the mother liquid will have formed crystals also. Filter this and combine with the first product, wait a couple of hours to make sure it has all crystalized.
**Solidifaction process skipped. See Cheapskate Write Up for details
Yield was 43 grams of white needle like crystals.
Making N-acetyl-anthranilic acid
1) In a 2 L + vessle add 1300ml of water and dissolve 20 grams of N-acetyl-o-toluidine and
50 grams of magnesium sulfate in it while stirring
2) Slowly raise temp to 80c to dissolve the N-acetyl-o-toluidine. This will take a few minutes. At 80c crystals should dissappear.
3) Add 50 grams of potassium permanganate, increase the stirring speed to keep the solution from settling.
4) Stir solution for 3 hours at 85-90c. Add water as necessary.
5) Neutralize solution with 30ml of denatured alchol. Solution should turn brown and pink fluid should
disappear. Add another 10ml of denatured alchol if solution is still pink.
6) Filter solution hot, with suction. Be sure to get as much of the solution as possible
7) While stirring ad 10% sulfuric acid a few ml at a time. The N-acetyl-anthranilic acid will precipitate out.
Filter and clean by dissolving in weak NaOH and reprecipitate by adding sulfuric as before.
Yield 16 grams N-acetyl-anthranilic acid
Making Methaqualone
Method 1.
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.
2) 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 mess with what is in the test tube!
3) Allow heating o-toluidine to dissolve all the anthranilic, turning it black. If some anthranilic remains undisolved tilt and swirl the test tube.
4) Over the next 30 min raise the temp of the test tube to 190c. Water will be evolved from the reaction creating bubbles. Hold temp for 3 hours. **
5) Add 2x the volume of acetone. Stir until purple stuff dissolves.
6) Allow acetone to cool or HCL will boil. Add same volume of 34% hcl as purple stuff.
7) Bring entier solution to boil for 4 minutes, remove hear and allow to cool.
Allow solution to cool for 1.5 hours, crystals will form in the purple stuff. If necessary refrigerate solution.
If no crystals form, heat a glob of purple stuff return it to the flask and stir.
9) Filter the crystals dry and proceed to purification!
Purification:
1) Dissolve crystals in beaker by boiling with 2x amount of Acetone & boiling stones.
2) Filter the crystals and dry.
~If, after drying, there is a purple tint to the crystals, then recrystalize from
methanol. Put crystals in a small beaker add enough MeOH to get them wet and start
heating the mix. If crystals don't dissolve bring the MeOH to a boil and add MeOH a little more,
boil until they have all dissolved. Boil until about 20% of the MeOH has been evaporated. Allow the
solution to cool and wait. Crystals will form in about an hour, 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 the solution and the crystals. ~
3) 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, wash with acdtone again.
4) Take purple solution you saved from recrystalization, add boiling granules and boil away half the volume.
5) Allow this to cool and methaqualone will precipitate. Purify with acetone as above(if necessary) and add 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.
Method 2.
(Skipped see Cheapskate Write Up)
Method 3:
(Skipped see Cheapskape Write Up)
Super purification:
1) 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, some stuff will not dissolve.
2) 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! WOOHOO! **
Yield
of (white??) methaqualone crystals