Maui3 - 21-12-2024 at 10:39
Important Note:
I know about Methaqualones uses as a recreational drug, but I am just making it because I think methaqualones history is quite interesting. I am NOT
going to ingest it, and I do NOT recommend anybody else do that either. I also chose to not tell say the quantities of the reagents I am using. I
mean, anyone with half a brain cell can find that on their own - it is actually the first result on google, but I still felt it was better to do it
this way. 
Short Introduction:
In short, methaqualone was invented as an alternative to barbiturates. Barbiturates being a class of sedative and hypnotic drugs, which at the time
often was prescribed to stressed mothers. Unfortunately, barbiturates actually made the stressed mothers addicted to the drug, and they
quickly built up a tolerance. The stressed mothers would sometimes go to different doctors to get multiple prescriptions of the barbiturates, so they
could get more than their recommended does. (I have no idea how that was even possible). Methaqualone was marketed under the name "Quaalude".
Quaaludes seemed promising at first, but people eventually figured out that if they stayed awake after taking the drug they got quite intoxicated.
According to one source, a tolerance to the drug could build up in less than a week if used recreationally, though I have not gotten that confirmed.
Quaaludes were very popular as partydrugs in the 70's and was even used by the famous singer - Elvis Presley. Eventually the government also found out
that.. well.. maybe Quaaludes weren't that great afterall, and they shut the sale of them down. Following that, Quaaludes became very rare. Today,
they are pretty much only made and used illegaly in South Africa. I have found a very good documentary about it from "Hamiltons Pharmacopeia" if
anyone is interested.
Please correct me if I said something incorrect, this was all just written from what I remember.
Legality:
Obviously methaqualone is now illegal, but it's analogues aren't! I found a very similar analogue with roughly the same effects, though a bit less
potent, that actually is relativily obscure. The analogue's obscurity actually suprises me a bit since it is just methaqualone with a methyl group
replaced by a ethyl group.
Short Note Before Synthesis:
This is pretty much identical to the normal methaqualone synthesis procedure, just with the o-toluidine being replaced by 2-ethylaniline to get the
ethyl analogue.
Synthesis of Phthalimide:
The phtalimide was synthesized from a mixture of urea and phthalic anhydride which was grounded in a mortar, heated to 140 C until it stopped foaming
(the foaming actually solidified), mixed with water and filtered. The filtercake containing the phthalimide.
Synthesis of Isatoic Anhydride:
I tried to directly synthesize anthranillic acid from phthalimide, but that reaction was a nightmare. I tried so many times, with different methods,
and it never wanted to work. So I reccomend this one instead.
There was prepared 3 solutions. Solution A being 2.5% sodium hypochlorite (bought as bleach), solution B being sodium hydroxide in water and solution
C being phthalimide, crushed icecubes and water. The 3 solutions were cooled to 0 C in an icebath. The sodium hydroxide solution was added to the
phthalimide solution with a addition funnel (still at 0 C).
TIP: Use addition funnel instead of pipette. If you use pipette, you start to get impatient and add it to quickly.
The mixture was cooled to 0 C again, and the 2% sodium hypochlorite was added also with additions funnel (still at 0 C). The mixture was let stir at
5-6 C for 15 minutes, whereafter the mixture was adjusted to pH 6 with conc. HCl.
NOTE: The procedure I was following said to let it stir for 90 minutes, but all of my isatoic anhydride crashed out and became a thick slurry, so I
decided to skip that step.
The mixture was then filtered, and the filtercake containing isatoic anhydride was washed with water.
Synthesis of Anthranillic Acid:
The isatoic anhydride was mixed with a aqueous solution of sodium hydroxide and let stand for 15 minutes. After the 15 minutes, conc. HCl was added
with a addition funnel VERY VERY SLOWLY, until the pH was around 4. After a day the mixture had still not precipetated any anthranillic acid, so the
mixture was boiled down on LOW heat, until the anthranillic acid started to precipetate. The mixture was cooled and the anthranillic acid was
collected.
Synthesis of Etaqualon (Quaalude Analogue) - Method A:
The anthranillic acid was dissolved in acetic anhydride, the mixture was heated to 200 C. The mixture was cooled to 60 C and 2-ethylaniline was added
in portions. The mixture was again heated to 200 C, and was supposed to be heated to 200 C at 2 hours, but not suprisingly it started to solidify, so
I just stopped the reaction there. After cooling to 100 C, diluted HCl was added CAREFULLY and the miture was boiled for 15 minutes. Thereafter the
mixture was neutralized with sodium hydroxide solution which made the etaqualone precipetate as oil. The oil solidified upon cooling and stirring. The
product melted at the right temperature, so I assume it is etaqualone.
Synthesis of Etaqualon (Quaalude Analogue) - Method B:
Some of the isatoic anhydride and 2-ethylaniline were refluxed in xylene for 90 minutes, after which acetic anhydride containing some HCl was added,
and refluxing was continued for another hour. The aqueous layer was reacted with NaOH and the etaqualone precipetated as oil. NOTE: I haven't tested
melting point on this method yet.