Methaqualone Scaleup

Procedure

150 ml of lab grade o-toluidine was placed in a 1 liter RBF and equipped with a condensor. 150 ml of acetic anhydride was stolen from a highschool chemistry storeroom and added to the toluidine at a rate that kept the exothermic rxn under control. Heat was added to keep reflux going for another 10 minutes, then the contents were dumped into a beaker with 2.5 liters of water. Light pink crystals formed immediately. It was put in the freezer for a couple of hours, and more precipitate had formed. Precip. was vacuum filtered, and air sucked through for awhile to speed drying. Precip. was now mostly white with only a hint of pink, so recrystallization was skipped. It was dryed in a vacuum dessicator with CaCl2 dessicant overnight, and the next day the weight of the dry N-acetyl-o- toluidine was 167.6 g.

Into a 20 liter jar with heating mantle was placed 11 liters of water, 167.6 g NAOT, 425 g MgSO4 and 425 g KMnO4 (350 g lab grade, and 75 g stuff for refilling water filters for removing iron). Heating was commenced and temperature held at 80 to 90°C for 3 hrs. Then 250 ml of ethanol was added to neutralize the KMNO4. Now for the dreaded filtration. This is impossible without celite (diatomaceous earth). Don't let chem supply places assrape you on the price of this, go to a pool/spa place and pick up a 20 pound back for $11. The nasty mud was vac. filtered through a layer of celite, and it worked out better than swim remembered. The solution was filtered again to clear it up some more. 5 gallon ozarka water bottles were used to handle the large volumes of liquids. 10% sulfuric acid was added to precipitate the N-acetyl anthranilic acid. The precipitate was filtered again, rinsed with clean water, sucked dry for awhile, and dried in a vacuum dessicator overnight. Yield of bright white crystals was 136.1 g.

136.1 g of NAAA was added to a 1000 ml RBF. 190 ml o-toluidine was added and heating commenced. The solution turned dark purple and water was evolved and boiled off. After a few hours, heat was removed and 160 ml 31% HCl and 300ml acetone were added. Boiling was commenced for a few minutes. It was removed from the heat and put in the freezer. The next day there still was no crystals so the acetone and water were rotovapped off. Fresh acetone (maybe 150ml) was added and boiling commenced. Upon cooling, crystallization commenced. It was put in the freezer for awhile,then filtered and washed with fresh acetone. Fluffy powder was bright white. The methaqualone was dried, and weighed 96.4 g.

Swim didn't like the texture of the powder, very fine, and it had a slight acetic smell to it, so it was added to a beaker of dilute NaOH and stirred for awhile. Then filtered. Filter cake was washed with fresh water, then recrystallized from dilute, boiling HCl solution. Crystals were filtered, rinsed, dried in vacuum desicator to weight of 66.7 g. It was bright white and sparkly. Individual crystals could be seen as tiny spicules. 10% H2SO4 was added to the dilute NaOH. Lots of NAAA precipitated, but it hasn't been filtered yet.

Overall, 150ml (1.4 mol) o-toluidine produced 66.7g (.27 mol) of methaqualone for an overall yield of about 20%. The permanganate oxidation was a bitch because of the large volumes. The NAAA/o-toluidine condensation is frustrating because yields are so low.

After recrystallization of the methaqualone.HCl, the mother liquor was saved in a glass container. Over the last 7~8 months, about half has evaporated, and more methaqualone.HCl precipitated out. Swim noticed recently, and filtered it, crunched up the crystals, rinsed with a little fresh H2O, then acetone, then dried. Weight is 9.5 grams of sparkly white methaqualone.HCl, and since about half of the mother liquor still remains, Swim is guessing that he'll be able to get out another 9 grams or so. So add another 18~19 grams to the overall yield of the above writeup. Yeah! I'm so happy! I really missed those quaaludes.

Oh yeah, Swim checked that it wasn't N-acetylanthranilic acid by adding a small amount of the powder to a beaker of warm NaOH solution. NAAA would react and dissolve, but methaqualone will slowly react to form the freebase, which is insoluble. The second action is what was observed. And the powder has the right solubility properties in room temperature acetone and water (not very soluble in either), the correct horrible taste, and it looks like the previous powder. (Very sparkly). Bioassay will gladly ensue tonight!

Bioassay is very pleasurable and definitely confirms the identity of this powder. Yeah!! I'm so happy! Much thanks to Cheapskate.