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Methaqualone
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􏂆
 (Quaalude) synthesis
 G.Patton ·  Jan 6, 2022

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 G.Patton
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Jan 6, 2022  #1


Introduction

In this topic, you can find chemical properties and synthesis pathway of
Methaqualone (Quaalude; 2-Methyl-3-(2-methylphenyl)-4(3H)-quinazolinone) from
isatoic anhydride and o-toluidine with high yield. These
 Log in precursor   are
Register substances 
quite common and do not attract a lot of attention. You can easily buy them in a
chemistry store at a good price. These methods are elementary and can be easily
scaled up. Don't forget about safety and use PPE.​

Equipment and glassware:

Pear-shaped flask 10-50 ml and 100 ml;

Buchner flask and funnel (or small Schott filter);
Heated magnetic stirrer;
Reflux condenser (small);
Retort stand and clamp for securing apparatus;
Laboratory scale (0.01 — 100 g is suitable);
Pasteur pipette's;
Water and oil bath;
Laboratory grade thermometer;
Vacuum desiccator (optional);
Water-jet aspirator (optional);
Beakers 100 ml x2; 50 ml x2; 10 ml x2;
Glass rod;
Boiling stones;
Conventional funnel;
 Filter paper.
 Reagents:

o-Toluidine 1.1 g, 0.01 mol;

Isatoic anhydride 1.6 g, 0.01 mole;

Diethyl ether (Et2O) or acetone and distilled water ~50 ml;
 Dichloromethane (CH2Cl2) 100 ml;
Petroleum ether 100 ml;
􏂆
 Acetylacetone 0.39 g, 0.0025 mole;
Ethanol (EtOH) 95% 30 ml;
 Hydrochloric acid conc. (HCl) ~10 ml;
Methanole MeOH 50 ml;​
 Acetone 50 ml.

Soluble in ethanol and ether. Insoluble in H2O;

Boiling Point: 406.9 °C at 760 mm Hg;
Melting Point freebase: 113-115 ̊C;
Melting point HCI salt: 235-237 ̊C;
Molecular Weight: 250.301 g/mole;
Density: 1.16 g/cm3 (20 °C);
CAS Number: 72-44-6.

Procedure
2,2'-dimethylbenzanilide (1)
A mixture of isatoic anhydride (1.6 g, 0.01 mole) and o-toluidine (1.1 g, 0,01 mol) is
heated in a pear-shaped flask (10-50 ml) to 120 °С for 2 hours with a small reflux
condenser in an oil bath. The reaction mixture after cooling is triturated with ether
(or dissolve the brown mixture in warm acetone and add water to crash out the
crystals). The resulting solid is collected by suction filtration on Buchner funnel (or
small Schott filter) and recrystallized from a 50:50 mixture of dichloromethane and
petroleum ether to give the intermediate aminoamide (2,2'-dimethylbenzanilide) (1):
yield: 1.7 g (75%); m.p. 110 °C.​




􏂆
 2-Methyl-3-(2-methylphenyl)-4(3H)-quinazolinone (2)
A mixture of 2,2'-dimethylbenzanilide (0.5 g, 0.0025 mole), acetylacetone (0.39 g,
 0.0025 mol) in ethanol (30 ml) containing a few drops of concentrated hydrochloric
acid is refluxed for 1 h in a pear-shaped flask 100 ml. On cooling the title compound

separated by filtration as the hydrochloride salt: yield: 0.59 g, (85%), m.p. 235-237
 °C.​


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 stones. They help the boil start
faster and stay under control. 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 recrystallize from methanol. To accomplish this, put the crystals in a
small beaker add just enough MeOH to get them wet and start heating the mix.
Some 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 recrystallization 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 recrystallization
will create a new surface, so an 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 gray 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 recrystallization above? This is nasty-
purple-stuff, MeOH, acetone and methaqualone. Put a few boiling stones 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
07 Jan #2
􏂆
 last acetone boil to clean it up.​
Aaaargh, you beat me to it. Last edited: Jan 17, 2022
But there are other routes starting with other materials. Often times the starting
 material will be something like toluene and methyl anthranilate or phtalic
Unclejoe007 and Superfly$$
anhydride. Or even vinyl gloves.
 MadHatter
Don't buy from me
Resident
I think the most elegant OTC route to this synth is toluene and methyl
 anthranilate.
Joined: Dec 4, 2021
Messages: 442 Toluene to be treated with nitrating mixture of sulphuric acid/nitric acid to yield
 Solutions: 1 racemic nitrotoluene, which is then easily separated through freezing points
Reaction score: 417 yielding o-nitrotoluene. The o-nitrotoluene is then refluxed over tin with addition
Points: 63
 of HCl to yield o-toluidine.
The methyl anthranilate is available as a fragrance/taste chemical from diverse
 vendors in the perfume industry. It can be demethylated easily through
treatment with NaOH to yield anthranilic acid, which can then be used together
 with the o-toluidine.

The problem with this drug is the high doses needed to achieve effect. A normal
dose is around 400 mg, which makes it difficult to break even. Also, the workups
a bitch, honestly, It's really difficult to achieve a pure, white end product.

Unclejoe007 and Nyarlothotep

The chef
Don't buy from me
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Joined: Jun 5, 2022 Messages: 7 Reaction score: 0 Points: 1

By The chef Jul 15, 2023  #21

where do i find the synthesis ?

07 Jan  #3

J isatoic anhydride condenses with o-toluidine to form 2-amino-N-(o-

tolyl)benzamide
http://linx4f75phtm63mxalb2wtspofcodku5lwofiyoupda4n4uc6cfjuzid.onion/p4
v2bmun.png
Jack
Don't buy from me Sci-Hub | Heterocyclic Compounds; IX. A Facile Synthesis of Meth…
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sci-hub.hkvisa.net
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Messages: 53
Reaction score: 18
Points: 8


 07 Jan  #4

The reaction looks simple, but it is a bit difficult to perform, the reaction is very
difficult to clean and you will lose a batch of glass instruments.
 o-toluidine is carcinogenic and very likely to cause bladder cancer and requires
good safety precautions.
Uncle Lee
 Don't buy from me
I don't think it is easy to synthesize pure o-toluidine, the best way is to buy the
New Member
substance (if you can)

􏂆
 Joined: Jan 1, 2022
Messages: 44
Reaction score: 51
Nyarlothotep, Hedgie and G.Patton
Points: 18


 07 Jan  #5

Really? What is the main problem with the synth in your opinion?

And yes, the methaqualone synth is messy, producing chocolate-like slurries, a

lot of smell and a long and difficult work-up with a lot of yield loss. Toluene is
MadHatter
Don't buy from me
better than acetone for purifying the crude mq.

Resident Last edited: Jan 7, 2022

 Joined: Dec 4, 2021

Messages: 442
Solutions: 1
 Reaction score: 417
Points: 63

07 Jan  #6

I know these ways. I described here the simplest way for low skill auditory.
Isatoic anhydride and o-toluidine can be bought in chemical shop.
Last edited by a moderator: Jan 8, 2022

G.Patton
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07 Jan  #7

o-Toluidine has approximately 200 deg. boiling point, it is not much volatile
liquid, but I agree with safety precautions.
Last edited by a moderator: Jan 8, 2022

G.Patton
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 08 Jan  #8

 In fact, I can buy o-toluidine, so I have no experience in producing this

substance, but when I talk to other chemists, they tell me that it is very
Uncle Lee
 Don't buy from me
troublesome to synthesize this substance because the reaction vessel is
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difficult to clean and the substance is toxic.

􏂆
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Messages: 44
Reaction score: 51
Points: 18


 08 Jan  #9


You are correct that it is not easy to inhale the vapors of this substance and
cause poisoning if safety measures are good, but ensuring that the final product

(Quaalude) synthesized by the chemist is free of toxic substances is difficult.
Uncle Lee
Don't buy from me
If the chemist uses the substance himself or lets others use it, he needs to

New Member
make sure that the product is very pure.

 Joined: Jan 1, 2022

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Reaction score: 51
 Points: 18

08 Jan  #10

Really? Because no chemists I have talked to has had any problems with this
synth, and neither have I. There is a very comprehensive video on youtube also,
so there's really no need for me to produce another:
I never found the cleaning of the glassware very difficult, just rinse with water,
MadHatter
Don't buy from me
NaOH and if needed some DCM or toluene. Although focused on the racemic
Resident
separation of p-toluidine through the intermediary use of oxalate, the video also
shows the synth of toluidine, and if the starting material was pure o-
Joined: Dec 4, 2021
Messages: 442 nitrotoluene, the product would be o-toluidine also.
Solutions: 1
Reaction score: 417
SEPARATION ISOMERS TOLUIDINE. #ncchem
Points: 63

.
The o-toluidine is smelly and toxic at prolonged exposure, but any real cook or
 chemist would do this in a fumehood anyway.
 But as for the methaqualone, I fully agree with the messiness. And the real work
in that synth is the cleanup, as is also mentioned in the original post. The "nasty
purple", or as often is the case, the nasty brown, is not acceptable and takes a
LOT of work to get rid off.
 There is an episode of Hamilton Morris' Pharmacopeia in which he investigates
the origins of methaqualone in South Africa (which is the only country where
 this drug is still in widespread use), and he meets with a clandestine cook who
prepares crude methaqualone in a backyard using very primitive techniques and
no PPE whatsoever. He tells Hamilton about how he sometimes urinate blood ...
􏂆

I wonder what the levels of bladder cancer is among methaqualone users there.


Last edited: Jan 8, 2022
madmoney69

09 Jan  #11

I admit I am not very good at this reaction, you seem to be very experienced
with this reaction, I have not synthesized o-toluidine, I was just talking to my
friend about Methaqualone being difficult in purification and that o-toluidine is
toxic, I said to him that potassium dichromate is also class one carcinogen and
Uncle Lee
Don't buy from me
we all use it regularly, my friend told me that o-toluidine is more dangerous,
New Member
especially if it is taken as an impurity in methaqualone.
Joined: Jan 1, 2022
Messages: 44
Reaction score: 51
Points: 18

09 Jan  #12

Since I was not interested in sedatives, I did not continue my research and
experiments, I just recounted what I talked to my friend and I apologize to you
for my lack of rigor.

Uncle Lee
Don't buy from me
My friend, who is in the pharmaceutical industry, told me that o-toluidine is
New Member
relatively dangerous and that every year, employees of chemical plants get
Joined: Jan 1, 2022
cancer from handling this substance because of poor safety measures, so
Messages: 44 anyone who synthesizes this substance needs to be more careful about safety
Reaction score: 51
Points: 18

 17 Jan  #13

I made Methaqualone starting with pthalic anhydride + urea to make anthranilic

acid and then combined that with o-toluidine and glacial acetic acid (that’s a
 really rough outline, but it’s what I remember off the top of my head) to get to
MQ, and I had fairly good success after work-up.
Hedgie
 Don't buy from me
I had a good friend give me some decent advice before I did the synthesis which
New Member
I credit with my success. His basic strategy was to obtain the purest starting
Joined: Jan 16, 2022
materials he could, making sure that the anthranilic acid used is pure (it’s a
􏂆

Messages: 10 white crystalline solid when pure), and to make sure that the o-toluidine is
Reaction score: 19 recently distilled, that it’s a clear pale yellow oil (typically when it comes from a
Points: 3
 commercial supplier it arrives as a dark red oil because it has been sitting
around for a while & for our purposes this is unacceptable, so we need to take
 the commercial o-toluidine and distill it just prior to using it in MQ synthesis).
Taking these steps prior to making it did seem to help create a reasonably clean
 product, although I did recrystallize the final product a couple times as well.
Methaqualone is a fairly straightforward synthesis, however, it is notoriously
 difficult to get all the impurities out so that it is completely safe for human use. I
think someone mentioned it above already but I’ll say it again; this stuff has a
 reputation for causing bladder cancer because of the impurities left over from
synthesis, so if you are going to be using it yourself or giving it to someone you
 should definitely take the time to make sure you start with the highest purity
compounds you can and do a solid work-up on the product.
 the money, madmoney69 and MadHatter

17 Jan  #14

Yes, the real work in this synthesis is actually before and after the synth itself.
Both anthranilic acid and o-toluidine has a tendency to dark up and become full
of impurities if they're not synthezised or stored with the outmost care. And
finally, so does the MQ itself.
MadHatter
Don't buy from me
When you did the conversion from phtalic anhydride to anthranilic acid, did you
Resident
manage to obtain a reasonably pale product or did it become dark and impure?
Joined: Dec 4, 2021
This is a very common problem, and I think its very much a question of careful
Messages: 442 preparation of the hydroxide/hypochlorite reaction mixture.
Solutions: 1
Reaction score: 417
Points: 63

17 Jan  #15

J This thread is inaccurate the first image at the top of the page is the molecule
Alprazolam, I should have been more specific but the post I made above was
that in the first step of the reaction 2,2' dimethylbenzanilide isn't produced
instead 2-amino-N-(o-tolyl)benzamide is produced (the amino group is not
Jack
Don't buy from me
converted to a methyl group.
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G.Patton
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
 17 Jan  #16

Sorry, loaded wrong pic. Fixed.


G.Patton
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
22 Jan  #17


M I've synthesized methaqualone many times, using anthranilic acid, o-toluidine,
polyphosphoric acid and glacial acetic acid. It's pretty easy, but the part where
you neutralize the mixture using carbonate..... disgusting. I mean, look at this
(attached).
 Midget_Impinger
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
Joined: Sep 10, 2022
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Points: 8

I tried it twice thinking this was a failure. Then someone on SM told me that I
should just continue, and it actually worked! lol.

Here's a good SM thread on it:

http://www.sciencemadness.org/talk/viewthread.php?tid=156723

MadHatter, madmoney69 and G.Patton

22 Jan  #18

M Also, does anyone get the annoying twitches when they take methaqualone? I
quit taking it because I program for a living, and it was making it very difficult.

Midget_Impinger
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
 25 Jan  #19

Where you guys get anthranilic acid as I see its banned in china
By Midget_Impinger
 M 29 Jan  #20
It's so easy to make.
madmoney69
 Don't buy from me
Resident
The easiest way is to get methyl anthranilate and react it with sodium

􏂆
 Language: 🇬🇧 hydroxide (here). Can you check and see if you can get methyl
anthranilate? It's the most common grape flavoring, and it's also used as
Joined: Jan 29, 2022
Messages: 164 a duck/goose repellent. But the problem with methyl anthranilate is that
Reaction score: 160
 it's an ester of anthranilic acid. so it may be difficult to get as well..
Points: 43

 So if you can't get methyl anthranilate, then you can make anthranilic
acid from phthalimide. Here are a few videos:


 Anthranilic Acid : Organic synthesis

Synthesis of Anthranilic acid from Phthalim…

Phthalim…


 anthranilic acid and the hofmann rearrange…
rearrange…

􏂆



https://www.bitchute.com/video/lt07v5I2lSEp/
https://www.bitchute.com/video/OxYgvew9P6DR/

And phthalimide isn't restricted at all (at least where I'm at it isn't). But if
 it is, just google "how to make phthalimide". It's made from phthalic
anhydride or phthalic acid, which is also easy to get.

Forums Synthesis Technologies and Analysis Other
If you need to take the long route, then take a look at this NileRed video.
 If you follow the first 30 minutes, you'll see how you can take vinyl
glovesaneroo
containing either DEHP or DINP as the plasticizer, and turn that
and madmoney69
  ABOUT US into anthranilic acid).

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