Sciencemadness Discussion Board

Methaqualone

Benignium - 11-12-2020 at 02:52

There is something delightfully attractive about things that are prohibited or otherwise challenging to obtain. Exclusivity. Perhaps the desire to feel special. I guess if you know you know. Oftentimes it is very motivating to work towards a product that you can't simply buy from any chemical supplier.

So here's me making drugs.

Reference.

9.63 grams of o-toluidine, 14.19 grams of anthranilic acid and 9.00 grams of glacial acetic acid were combined in a 250 mL Erlenmeyer. With strong stirring, 90 grams of hot polyphosphoric acid was added in 10-20 gram portions using a glass syringe. The mixture was heated to and kept at 185 degrees Celsius for three hours.

Degraded, stored-for-a-while o-toluidine.


PPA <--> o-T + AA


After adding all of the PPA.


Reaction taking place.


Cooled reaction mixture.


Once sufficiently cooled, the reaction mixture was poured in 400 mL of water and, after filtration, the solution was made basic using sodium carbonate. A grotesque mass separated from the aqueous solution and floated to the surface. The liquid was discarded and the solid(ish) mass melted and dried in the oven at 110 deg. C. This was then dissolved in in acetone and sufficient concentrated hydrochloric acid was added to precipitate out the product as the hydrochloride salt.

Reaction mixture being poured in water.


Some initial garbage caught in the filter.


Apparently, some people consume and even smoke this stuff.


Melted and sufficiently dry.


Precipitate containing crude methaqualone hydrochloride.


The crude product was collected by vacuum filtration and dried. At this point it looks deceivingly clean and weighs 9.63 grams. The solid was dissolved in minimal methanol, filtered and dried. Once dry the solid was washed with anhydrous acetone. This was then dissolved, dried and washed two more times in the same manner.

Crude product vacuum filtered.


Crude product dried.


Impurity exposed after redissolving and drying.


The now cleaner product was dissolved in acidified boiling water and treated with activated charcoal. There was some improvement. The treated solution was made basic, filtered and the solid base dried. The melting point range was determined to be 106-110 deg. C according to an interrupted alcohol-based thermometer. Actual melting point was likely a few degrees higher.

Product being dissolved in acidic water.


Hydrochloride solution before charcoal treatment.


Hydrochloride solution after charcoal treatment.


Methaqualone base.


Melting point test.


Melting point test. Still impure.


The product was once more converted to its hydrochloride salt. Recrystallization from the aqueous solution was attempted revealing more garbage. The solids were washed with acetonitrile, whose performance was very similar to that of acetone, dissolved in methanol, dried and washed with acetone.

Hydrochloride recrystallized from acidic water.


Getting there.


Finally, when no more color seemed to come off with acetone, the product was dissolved in minimal boiling methanol. An equivalent volume of MEK was added and much of the methanol was boiled off. At about the original volume of methanol, the still clear solution was taken off heat and a dash of acetone was added. This method of recrystallization is somewhat unreliable but affords decent crystals.

No matter what I tried - and I tried a lot of different things - some color always remained. Here are some of the purest crystals I could manage:






The whole project was a bit of a mess but I am still immensely happy with the fact that I managed as well as I did. All the reagents for this project, except for the phthalic anhydride which I purchased off Ebay, were sourced OTC which makes it all that much more special to me.

And now for a small rant. The workup was extremely frustrating. There was an incredible amount of colored impurity that followed the product everywhere and had to be leached out bit by bit. This is all well and good, but methaqualone has an incredibly obnoxious tendency to dissolve in solvents that it isn't soluble in if there is even a drop of water, alcohol, etc. in them. This makes it really hard to purify everything as you often have to go back a step and reclaim whatever you lost to unexpected dissolution. I might revisit the preparation and workup at a later date to see if using cleaner reagents and utilizing acetic anhydride makes for a cleaner product. For now, though, I've definitely had enough.




[Edited on 11-12-2020 by Benignium]

mackolol - 11-12-2020 at 09:14

Generally this forum is not about drug making. It's even prohibited to do it here. There may be some exceptions if it actually teaches something about chemistry. I'm curious how will admins react to this. I like the workup though. It's great

stoichiometric_steve - 11-12-2020 at 09:22

Of course the subject of this post is a scheduled substance, but nonetheless the presentation is far beyond anything cookery related.

Great presentation, Benignium. Thanks for sharing!

Corrosive Joeseph - 11-12-2020 at 09:38

Quote: Originally posted by mackolol  
It's even prohibited to do it here.


This is not technically true.... Drug chemistry is acceptable, as long as it is discussed in a scientific manner.
I actually think the OP has done excellentl here and has provided a well done and tasty write-up.

Ludes went out of fashion with flares and platform shoes (the first time), I don't think anybody would be particularly interested in consuming the goods, or at least they shouldn't be.



/CJ

mackolol - 11-12-2020 at 09:50

Quote: Originally posted by Benignium  

The crude product was collected by vacuum filtration and dried. At this point it looks deceivingly clean and weighs 9.63 grams. The solid was dissolved in minimal methanol, filtered and dried. Once dry the solid was washed with anhydrous acetone. This was then dissolved, dried and washed two more times in the same manner.
[Edited on 11-12-2020 by Benignium]

I don't really understand this part, you have a HCl salt at this point and you said that you dissolved it in methanol. And then you just filter it from what? Do you mean recrystallisation or suspending it to wash the crude salt with methaqualone?

I wonder if it could be purified with good old A/B extraction though. Dissolving the salt in water and washing it with DCM. This shit works almost every time. Not sure about these type of compounds.

mackolol - 11-12-2020 at 09:57

Quote: Originally posted by Corrosive Joeseph  


Ludes went out of fashion with flares and platform shoes (the first time), I don't think anybody would be particularly interested in consuming the goods, or at least they shouldn't be.
/CJ

I wonder why. It's so easy to make them, yet practically nobody does so.
Of course there are now lots of different benzos and they're even legal (prescription drugs) and easily accessable. But I would always think of qualuudes as about this original drug producing big euforia, very addictive, irreplaceable. That's how they're described at least.

morganbw - 11-12-2020 at 10:03

OP
Quality post sir. Thank you.

Corrosive Joeseph - 11-12-2020 at 10:19

Quote: Originally posted by mackolol  

I wonder why. It's so easy to make them, yet practically nobody does so.


I can only guess, but if there was a demand, somebody would be filling it. They are a historical curiosity and I don't think many of todays youngsters have even heard of them.



/CJ

mackolol - 11-12-2020 at 10:25

Unless they've watched wolf of wall street :D

Pumukli - 11-12-2020 at 12:34

Some real work done. Sweet. :-)

A few remarks:

- A reaction equation would have been nice.

- How thoroughly could you check the properties of the target compound? Do you know its solubility in various solvents? Could it be e.g. steam distilled? Sublimated? (You mentioned people used to smoke it. Well, it may be a good candidate for sublimation.)

- Have you tried to remove the colourful contamination with something slightly polar (pentane/hexane/diethylether/whatnot) ? If they worked: great, if not: not a big deal, they evaporate quickly and don't interfere with the later stages of purification.

- What is the melting point of the pure methaqualone? How the various "semi-purified end products" converged to this value?

- I don't even mention TLC. :-)

All in all, the synth was very interesting, I could almost "feel" the pain of some of its stages based on the appearance of things on the photos.



[Edited on 11-12-2020 by Pumukli]

Amos - 11-12-2020 at 13:12

I'd love to know what your method for producing polyphoshoric acid is, and where you choose to stop the heating and finally use it. This is a reagent I'd love to try in a lot of different syntheses, particularly in inorganic chemistry.

Also, can I assume you made the o-toluidine the usual home chemist way by mono-nitrating toluene, reducing everything with a metal and acid, then steam-distilling?

Beautiful pictures and some very good chemistry on show in this post. This is the kind of scheduled substance post I can actually get behind.

itsallgoodjames - 11-12-2020 at 16:26

Great presentation! ( I don't intend on repeating this), but very informative and well presented.

Unrelated to anything, but the first image of the o-toluidine looks kind of like mercury if you don't look at it too closely

karlos³ - 12-12-2020 at 11:03

Very good publication!
But why haven't you put this into prepublication directly?
It is more than worthy for this.

Also, a personal opinion, I consider the product rather boring and would always prefer thalidomide to which I grew a certain fondness over time :)
This does also not have the certain possible impurities that ruin the experience with their harmfulness... bladder cancer is a big issue with clandestinely produced methaqualone or so, I've heard.
Due to possible toluidine residues.

It might make for an interesting next project for you to try the preparation of thalidomide?

aromaticfanatic - 12-12-2020 at 12:38

Quote: Originally posted by Amos  
I'd love to know what your method for producing polyphoshoric acid is, and where you choose to stop the heating and finally use it. This is a reagent I'd love to try in a lot of different syntheses, particularly in inorganic chemistry.

Also, can I assume you made the o-toluidine the usual home chemist way by mono-nitrating toluene, reducing everything with a metal and acid, then steam-distilling?

Beautiful pictures and some very good chemistry on show in this post. This is the kind of scheduled substance post I can actually get behind.

There is also a DCM nitration route to making almost purely o-nitrotoluene. Chemplayer has a video on it and it is a very interesting reaction in my opinion. I wish there was a similar way to get the para product since I would prefer p over o for a benzocaine synth. I failed isomer separation last time due to lack of equipment that I wanted to dirty :I

zed - 14-12-2020 at 14:49

Yup. Once upon a time, I might have done such a thing. Not now.

There was a time, when purification of the final product, might have been easy.

That time, was before, you started the reaction sequence.

Simple vacuum distillation of your crude O-toluidine, should have delivered a more-or-less colorless starting material. And, probably a less colorfully contaminated product.

Also, of interest.... I have used PPA on occasion. Depending on reaction conditions, it may produce cruddy
charred-like products. Can other, milder reagents, perform your cyclization?

Amos. PPA is expensive, and not generally over the counter available.

The question is: What is PPA?

Well, it is dehydrated, or "Polymerized" Phosphoric Acid.

Seems to me, you can formulate a reasonable grade of PPA by microwaving phosphoric acid under vacuum.

Or, adding Phosphorus Pentoxide to Phosphoric Acid.

There might be some discussions found, in Pre-publication.

Maybe 5 to 10 years ago? I'll check......

OK, I found a link.....

https://www.sciencemadness.org/whisper/viewthread.php?tid=73...



[Edited on 15-12-2020 by zed]

[Edited on 15-12-2020 by zed]

[Edited on 15-12-2020 by zed]

arkoma - 14-12-2020 at 15:13

Man. Memories memories. In my high school daze we called 'ludes Gorilla biscuits. I've eaten the RORER ludes, before Lemmon bought them. (I'm 57)

And yes, very nice write up.

Corrosive Joeseph - 14-12-2020 at 16:43

Quote: Originally posted by zed  


OK, I found a link.....

https://www.sciencemadness.org/whisper/viewthread.php?tid=73...




Very cool..... I presume this also works with diammonium phosphate, or at least it should, very readily available as yeast nutrient at the brew shop.


/CJ

Uvxtal76 - 19-12-2020 at 22:38

Quote: Originally posted by karlos³  
Also, a personal opinion, I consider the product rather boring and would always prefer thalidomide to which I grew a certain fondness over time :)
This does also not have the certain possible impurities that ruin the experience with their harmfulness...


Thalidomide: As in the substance which caused this? https://helix.northwestern.edu/article/thalidomide-tragedy-l...

thors.lab - 21-12-2020 at 17:08

Excellent synthesis. The fact that this is all mostly OTC makes me question why street methaqualone is not more common than it is.

aromaticfanatic - 21-12-2020 at 18:45

Quote: Originally posted by thors.lab  
Excellent synthesis. The fact that this is all mostly OTC makes me question why street methaqualone is not more common than it is.


Likely due to it just being a virtually extinct drug. Plus continuous users would be at high risk for bladder cancer since most street level cooks will just half ass the entire thing and leave loads of o-toluidine impurities in there. Plus I am sure that the majority of people don't want to go through the entire trouble of making anthranilic acid from scratch, then making o-toluidine from scratch, buying or making (I rarely hear of success and never see a true write up) polyphosphoric acid, and then they have that super messy reaction to go through, AND to top it off there is likely loads of impurity issues that need to be resolved on top of that.

Just doesn't seem to be a fun type of thing overall.

Benignium - 27-12-2020 at 13:36

I would like to thank everyone who replied! I'm incredibly grateful for the positive response.

mackolol - To be frank I wasn't really too sure of this myself, but my interpretation was such that as long as my focus is on the chemistry it would be fine. I wish to keep posting here but in the future I will no longer make it as obvious if the subject is controversial. I've grown very attached to Sciencemadness and I would hate to do it harm.

As for your question, and I'm truly sorry it took me so long to get around to replying, the filtration in question was done just to get rid of any insoluble impurities that may be present.

I actually did try out the A/B approach but the line of inquiry took me a long time to finish. It worked out quite well and could in fact be used to significantly cut down on labor.

To some of the crude hydrochloride that was precipitated from acetone and redissolved in methanol, an approximated slight excess (2 grams) of oxalic acid dihydrate was added. The solution was concentrated for as long as it remained clear and water was added until no more precipitation was observed. The solution was decanted off and filtered. Dark brown solids remained in the beaker and on adding NaOH it was evident that no methaqualone was present.




The filtered solution was extracted once with 10 milliliters of DCM, which turned out to be enough to extract very nearly everything. The extract was stripped of solvent, redissolved in water and the aqueous solution made basic. Methaqualone base was filtered off and washed with water. The solid was dissolved in water by adding 48% hydrobromic acid dropwise. The water was removed by evaporation and the solid hydrobromide salt was recrystallized from minimal boiling methanol.



The hydrobromide salt seems to crystallize more readily and with significantly less impurity, affording very pale crystals even from a strongly colored mother liquor.

Pumukli - Steam distillation is a brilliant idea! I will definitely try it some day. Different melting points are reported for methaqualone ranging from 113 (Wikipedia) to 120 (PubChem) deg. Celsius. I have since repeated the melting point test with a proper thermometer and it seems consistent, with a sharp melting point range at 113-116. TLC plates are something I've been meaning to buy for ages now, but since it has not really been necessary until recently, I've just kept putting it off. Definitely going to need TLC going forward. Thank you!

Amos - I actually made a small post on the preparation of PPA. Perhaps you have already found it, but in any case here you go! You're absolutely correct on the o-toluidine - I followed ChemPlayer's procedure.

karlos³ - Thank you so much! I'm going to have to look into the prepublications as I'm still unfamiliar with the concept. I like the idea of synthesizing thalidomide. I recently learned that thalidomide very nearly made it so I would not be born. It is an interesting compound.




[Edited on 27-12-2020 by Benignium]

SuperOxide - 8-1-2021 at 13:24

Deleted - I asked about TLC, but I see you already answered that in your reply to Pumukli. Sorry :-) Ignore this.

[Edited on 8-1-2021 by SuperOxide]

mackolol - 9-1-2021 at 03:19

All right, one more example, that proves universality of A/B extractions.
It's good to do it, because of what Karlos have said about the toluidine impurities. Nobody wants to poison themselves, right?

SuperOxide - 17-1-2021 at 10:00

Quote: Originally posted by Benignium  

Degraded, stored-for-a-while o-toluidine.

How long did you store the o-toluidine for in order for it to degrade this much? I plan on making some o-toluidine, but I may not be able to use it for a while, so if it degrades that quickly then perhaps I should wait til I can work on the project for a few consecutive days in a row.
Also, did you purify the degraded o-toluidine before you used it? Or did you use it as is?

[Edited on 17-1-2021 by SuperOxide]

Tsjerk - 17-1-2021 at 11:28

I believe the salts of toluidine are stable, so you could form for example the HCl salt and store it as a water solution. Before use you then freebase it, extract with a solvent, dry with sodium sulfate and evaporate the solvent.

SuperOxide - 17-1-2021 at 11:33

Quote: Originally posted by Tsjerk  
I believe the salts of toluidine are stable, so you could form for example the HCl salt and store it as a water solution. Before use you then freebase it, extract with a solvent, dry with sodium sulfate and evaporate the solvent.

Ahh, ok. Good tip!


@Benignium - I have two questions:

1) What was your yield? You said you started with 14.19g of anthranilic acid and 9.63g of the o-toluidine. How much of the end product did you get on the other end? (Sorry if you mentioned this in an above post, I didn't see it though).

2) You said you started from OTC chemicals, does that mean the toluene you got was just a paint thinner/solvent? (Like the Klean Strip Toluene?) If so, did you nitrate it as it was, or did you do anything to clean it up or dry it first? I have some and I wasn't sure if I should go through the trouble of distilling it then trying to pull as much water out as possible, or if I could nitrate it as it is.

[Edited on 18-1-2021 by SuperOxide]

zed - 18-1-2021 at 02:19

Question about Toluidine degradation.

Freshly opened bottles of Aniline and Phenyl Hydrazine, contain a product that is colorless to yellowish, this product discolors quickly once the bottle has been opened.

Exposure to oxygen, I suppose.

When you revisit this bottle a few weeks later, the contents will be reddish, or reddish brown (though still clear). I can imagine a small amount of Toluidine in a fairly large bottle (lots of oxygen) could develop a molasses-like appearance pretty quickly.

Tsjerk - 18-1-2021 at 04:01

Yes, it is indeed oxygen which causes the coloring.

SuperOxide - 18-1-2021 at 06:18

Quote: Originally posted by zed  
Question about Toluidine degradation.

Freshly opened bottles of Aniline and Phenyl Hydrazine, contain a product that is colorless to yellowish, this product discolors quickly once the bottle has been opened.

Exposure to oxygen, I suppose.

When you revisit this bottle a few weeks later, the contents will be reddish, or reddish brown (though still clear). I can imagine a small amount of Toluidine in a fairly large bottle (lots of oxygen) could develop a molasses-like appearance pretty quickly.

Quote: Originally posted by Tsjerk  
Yes, it is indeed oxygen which causes the coloring.


I figured it was either O2 or UV causing the degradation. I have some N2 gas left in a container, perhaps when I create the o-toluidine I'll put it in the smallest possible bottle, then try to fill the dead space with the N2.
I plan on creating some phenol as well, so I may do the same thing to that.

Tsjerk - 18-1-2021 at 07:20

Phenol isn't air sensitive is it? Phenolates are though.

njl - 18-1-2021 at 07:52

I though phenol was air/uv sensitive with respect to polymerization?

Benignium - 18-1-2021 at 11:18

SuperOxide, I have no accurate yield to report. I started out with 9.63 grams of the crude. Beside impurities, a lot of the material ended up being tossed while investigating solubility and different methods of purification. Right now I have well over two grams of completely colorless material that I'm trying to get to form nice crystals.
The toluene is from a hardware store thinner. Fortunately for me it is quite pure - I have even made tosylic acid without much discoloration in the final product. I would highly recommend distillation as well as drying or separating any azeotrope, even if the MSDS states toluene as the only ingredient. However, some water isn't going to affect this particular nitration.

Thanks to zed, I figured out how to remove the remaining coloration. Treating the solution of methaqualone base in toluene seems to be the ticket here. It does not remove everything straight off the bat, however, and forming the hydrobromide salt after an A/B treatment using oxalic acid and recrystallizing it from methanol seems to be the most reliable way to get there.




mackolol - 18-1-2021 at 11:58

Quote: Originally posted by Benignium  

Thanks to zed, I figured out how to remove the remaining coloration. Treating the solution of methaqualone base in toluene seems to be the ticket here. It does not remove everything straight off the bat, however, and forming the hydrobromide salt after an A/B treatment using oxalic acid and recrystallizing it from methanol seems to be the most reliable way to get there.

This reminded me of purification of anthranillic acid thread. I don't really know the solubility of methaqualone freebase in hydrocarbons such as heptane, nor can I find it, but this can be solution for removing the remaining coloration: https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

Benignium - 19-1-2021 at 10:25

I did actually try something like that. As the amount I was working with was too small for my only soxhlet apparatus, I folded a basket out of coffee filter, loaded it with a paste of methaqualone paste mixed with some sodium carbonate and suspended it over boiling 60-90 petroleum ether, under reflux. I let it go for 24 hours or so. The methaqualone did indeed accumulate on the bottom of the boiling vessel, but so did some of the brown color. The extracted material was a clear, exceedingly tough gel with a brown tinge. The filter paper was- Actually, I believe I have pictures...










[Edited on 19-1-2021 by Benignium]

SuperOxide - 19-1-2021 at 15:38

Quote: Originally posted by Benignium  
The toluene is from a hardware store thinner. Fortunately for me it is quite pure - I have even made tosylic acid without much discoloration in the final product. I would highly recommend distillation as well as drying or separating any azeotrope, even if the MSDS states toluene as the only ingredient. However, some water isn't going to affect this particular nitration.

Right, I figured I should perhaps purify it using sulfuric acid to get rid of the thiophene contamination that's common with toluene, then distill it to get rid of as much water as possible.

Tsjerk - 23-1-2021 at 05:58

Quote: Originally posted by njl  
I though phenol was air/uv sensitive with respect to polymerization?


I was still wondering about this and had a quick search, I'm pretty sure it is only sensitive to light, maybe it oxidizes in air under the influence of light.

SuperOxide - 30-1-2021 at 07:56

I know in your PPA synth thread you mentioned that it etched away at the glass. Did that happen here as well in any step? You said you added the hot PPA (hot hot?), did the reaction vessel get etched away at all?

Benignium - 1-2-2021 at 14:34

No, not at all. The etching is only significant at temperatures exceeding 200 deg. C, possibly even 250.

On an unrelated note, I neglected to mention that the way I got rid of the last bit of color was by treating in toluene with activated carcoal. I should really learn to proofread my stuff properly.

SuperOxide - 1-2-2021 at 15:15

Quote: Originally posted by Benignium  
I neglected to mention that the way I got rid of the last bit of color was by treating in toluene with activated carcoal. I should really learn to proofread my stuff properly.


I wonder if that would be enough to purify it without having to go through some of the various purification steps you mentioned you tried, some of which seem tedious or repetitive. Perhaps just treat it with activated charcoal in toluene, then recrystallize it using methanol.

I hope to get to try this in the near future. I have everything needed for it now, except for time and space :(

Benignium - 1-2-2021 at 17:44

It wasn't quite that easy for me at least. A couple of methanol-acetone cycles, A/B using oxalic acid and finally charcoal is the minimum amount of workup you're looking at. That is unless you start with less impurities or figure out a better method. There's also no shame in settling for a slightly impure product as long as you're happy. Just don't consume it.


Amos - 1-2-2021 at 18:27

Benignium, thank you so much for keeping up with the thread and addressing all of the comments with such thoroughness. There are some qualities that have been lacking on forum posts of late and it looks like some of us are happy to see them freshly embodied here.

If you want to answer yet another question: When you say solvent/water was removed by evaporation, do you mean simply leaving a solution out to naturally concentrate, or are you assisting the process with a vacuum or other means?

Benignium - 2-2-2021 at 00:40

I appreciate the kind words, Amos! :)

Whenever there is the possibility of speeding up the process without the risk of losing product, I tend to go for it. I haven't utilized vacuum all that much thus far because my equipment lacks the necessary protection. Mostly I just heat the mixture near, or all the way to, its boiling point using either an oven, a water/oil bath or just a hotplate. I've also used PC fans to further encourage evaporation but lately that has fallen out of favor for no particular reason.

With all that said, I suspect the methaqualone may actually slowly break down into something yellow. The best indication of this was when converting colorless methaqualone base in toluene into the hydrochloride salt using hydrochloric acid while also applying heat. Of course, given that melting point tests are generally the most advanced analytical method in my arsenal, I cannot reasonably rule out the possibility of remaining impurities being the culprit.

SuperOxide - 2-2-2021 at 05:57

Quote: Originally posted by Tsjerk  
Phenol isn't air sensitive is it? Phenolates are though.

It definitely does degrade. Though apparently adding small amounts of HCl will help slow that down by a factor of 100 (approx).

https://lclane.net/text/phenol2.html

Wonder if that would work with o-toluidine...

njl - 2-2-2021 at 06:37

The salt is probably more stable than the freebase.

SuperOxide - 4-2-2021 at 10:47

@Benignium - in your initial post here, you said:
Quote: Originally posted by Benignium  
[...]

9.63 grams of o-toluidine, 14.19 grams of anthranilic acid and 9.00 grams of glacial acetic acid were combined in a 250 mL Erlenmeyer. With strong stirring, 90 grams of hot polyphosphoric acid was added in 10-20 gram portions using a glass syringe. The mixture was heated to and kept at 185 degrees Celsius for three hours.

[...]

However, in the Rhodium article you referenced, in the From Anthranilic Acid (Klosa) section you've used, it states:
Quote:
[...] After this, the mixture was heated to 180°C for 10 minutes, then cooled and poured in 150-200ml water, [...]

Which leaves me with a few questions:

  1. Is there any reason you went for 3 hours when the article says only 10 minutes is needed?
  2. Was there a noticeable change in the reaction flask that signaled the end point?
  3. Is there any risk of going for such a long time? (eg: more side products being created, leaving to an overly contaminated product)


Sorry if I'm hassling you with so many questions, hope it's not too much trouble.
As always, thanks for keeping up with the replies to the thread.

SuperOxide - 28-3-2021 at 17:00

Quote: Originally posted by karlos³  
[...]
Also, a personal opinion, I consider the product rather boring and would always prefer thalidomide to which I grew a certain fondness over time :) [...]


You prefer thalidomide? As in recreationally? Interesting... I didn't know it had any desirable effects.

Edit: I guess there is some market for it, very surprising. Found this thread on it's synthesis here.

[Edited on 29-3-2021 by SuperOxide]

SuperOxide - 2-5-2021 at 17:02

Thought I'd add some input to this suggestion:
Quote: Originally posted by Pumukli  
[...]

- How thoroughly could you check the properties of the target compound? Do you know its solubility in various solvents? Could it be e.g. steam distilled? Sublimated? (You mentioned people used to smoke it. Well, it may be a good candidate for sublimation.)

[...]

I was able to get this MQ synthesis a go as well (worked a treat thanks to OP's detailed post. So much in there that's not detailed anywhere else).

I decided to try the sublimation that was suggested by Pumukli. I took some photos of the process
Note: This was my first vacuum sublimation, so it's a rather sketchy setup, be gentle in your critiques, lol.

Summary: It does work ok. The crystals weren't nice and white like I was hoping, but they were definitely better than the crude product. Probably would have worked better with a higher vacuum and a better distributed heat source (eg: heating mantle instead of flame that needed to be moved around).

Here's a few of the photos of the crystals that sublimated onto the test tube:



[Edited on 3-5-2021 by SuperOxide]

Benignium - 3-5-2021 at 12:41

Thank you for trying the sublimation, SuperOxide! Very nice to see that it works.

For resizing the embedded image, I recommend augmenting the BBCode: [img] -> [img=16x9] -- so width x height given in pixels.



SuperOxide - 3-5-2021 at 12:57

Quote: Originally posted by Benignium  
Thank you for trying the sublimation, SuperOxide! Very nice to see that it works.

For resizing the embedded image, I recommend augmenting the BBCode: [img] -> [img=16x9] -- so width x height given in pixels.



Thanks! I modified the previous post to show a few of the pictures.

Perhaps sublimation of the base then using A/C in toluene is the way to go. Sublimation clearly gets rid of a lot of black residue (assuming carbon), but the crystals are still colored, hence the A/C.

[Edited on 4-5-2021 by SuperOxide]

SuperOxide - 5-5-2021 at 11:05

Quote: Originally posted by Benignium  
Thanks to zed, I figured out how to remove the remaining coloration. Treating the solution of methaqualone base in toluene seems to be the ticket here. It does not remove everything straight off the bat, however, and forming the hydrobromide salt after an A/B treatment using oxalic acid and recrystallizing it from methanol seems to be the most reliable way to get there.





Also thanks to Zed, I tried the same thing, and it seemed to work out perfectly.


It's not 100% white, it has a very small hint of yellow if you look at it at the right angle or under the right light, but it's by far the best I've done yet.

[Edited on 5-5-2021 by SuperOxide]