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All 3 posts Subject: Synth of a methaqualone analogue Please login to post Down

josef_k
(Hive Bee)
11-06-03 19:28
No 469185
      Synth of a methaqualone analogue
(Rated as: good read)

This is what i did:

6.4g (0.04mol) isatoic anhydride and 6.1g (0.04mol) 4-methyl-2-nitroaniline was put in a 100ml flask and heated to 120C. At that temp the 4-methyl-2-nitroaniline melted. But after a while the contents seemed to solidfy again, so I had to raise the temp more and more. I kept it on the heat for 2 hours. I noticed that some yellow crystals were crystallizing in the neck of the flask. After the 2 hours I dissolved the residue in acetone and added water to crash out the brown crystals. I should probably have recrystalized them, but I had no pet. ether mad , so they just had to do without. They weighed 12g (0.044mol) which is pretty unreasonable. I just assumed that it was really 0.03mol.

Then I put the crystals + 3g acetyl acetone and 6ml 30% HCl into 35ml ethanol/methanol and refluxed it for 1 hour. There was some bumping which was annoying. After it had cooled and I filtered the crystals I got 7g of some beige colored crystals. I tried to recrystalize them from ethanol, and after that they weighed 5g but were still beige and probably pretty unpure.

To test them out I first took 60mg, and after an hour 60mg more. Then I felt very mildly sedated. Next day I took about 800mg and then I felt more sedated. But the crystals must be VERY unpure since this analogue is supposed to be 5x regular methaqualone.

Next time I will get me some pet. ether and recrystallize the intermediate. And I think perhaps I should run the first reaction in some solvent, as I think that because I had to turn up the heat so much maybe ruined the yield.
Anyone have any other ideas on where i screwed up?

The method I used is described here: https://www.rhodium.ws/chemistry/quaalude.html.
And the analogue is described here: Patent US3162634.

toad
(Stranger)
11-13-03 18:10
No 470677
      Synth of a methaqualone analogue
(Rated as: excellent)

Hi Bees,

Just another toad tid bit to help fellow bees avoid any
dead ends that have been tried before. targets
were selected from several journal articles
(only have ref for one of them easily handy at the moment),
pharm and animal testing looked extremely promising,
but unfortunately all 3 compounds made and tested turned
out to be no go in humans. all were tried up to
very high amounts with little to no effects noted.
materials were verified with nmr and gcms so dont
think the synth was the problem.

Compound # 22 in JMedChem 1979, Vol. 22, No1,
2-(Fluoromethyl)-3-(o-tolyl)-4(3H)-quinazolinone

and

{2-methyl-3-(2,4-dimethylphenyl)-4-quinazolone}

and

{2-methyl-3-(4-ethylphenyl)-4-quinazolone}

still dreaming of analude xmas...

cheers,

toadie

Antoncho
(Official Hive Translator)
08-20-04 12:48
No 526463
      Another interesting one

Patent US3406173

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	All 3 posts		Subject: Synth of a methaqualone analogue		Please login to post		Down


		josef_k (Hive Bee) 11-06-03 19:28 No 469185				Synth of a methaqualone analogue (Rated as: good read)
						This is what i did: 6.4g (0.04mol) isatoic anhydride and 6.1g (0.04mol) 4-methyl-2-nitroaniline was put in a 100ml flask and heated to 120C. At that temp the 4-methyl-2-nitroaniline melted. But after a while the contents seemed to solidfy again, so I had to raise the temp more and more. I kept it on the heat for 2 hours. I noticed that some yellow crystals were crystallizing in the neck of the flask. After the 2 hours I dissolved the residue in acetone and added water to crash out the brown crystals. I should probably have recrystalized them, but I had no pet. ether , so they just had to do without. They weighed 12g (0.044mol) which is pretty unreasonable. I just assumed that it was really 0.03mol. Then I put the crystals + 3g acetyl acetone and 6ml 30% HCl into 35ml ethanol/methanol and refluxed it for 1 hour. There was some bumping which was annoying. After it had cooled and I filtered the crystals I got 7g of some beige colored crystals. I tried to recrystalize them from ethanol, and after that they weighed 5g but were still beige and probably pretty unpure. To test them out I first took 60mg, and after an hour 60mg more. Then I felt very mildly sedated. Next day I took about 800mg and then I felt more sedated. But the crystals must be VERY unpure since this analogue is supposed to be 5x regular methaqualone. Next time I will get me some pet. ether and recrystallize the intermediate. And I think perhaps I should run the first reaction in some solvent, as I think that because I had to turn up the heat so much maybe ruined the yield. Anyone have any other ideas on where i screwed up? The method I used is described here: https://www.rhodium.ws/chemistry/quaalude.html. And the analogue is described here: Patent US3162634.



		toad (Stranger) 11-13-03 18:10 No 470677				Synth of a methaqualone analogue (Rated as: excellent)
						Hi Bees, Just another toad tid bit to help fellow bees avoid any dead ends that have been tried before. targets were selected from several journal articles (only have ref for one of them easily handy at the moment), pharm and animal testing looked extremely promising, but unfortunately all 3 compounds made and tested turned out to be no go in humans. all were tried up to very high amounts with little to no effects noted. materials were verified with nmr and gcms so dont think the synth was the problem. Compound # 22 in JMedChem 1979, Vol. 22, No1, 2-(Fluoromethyl)-3-(o-tolyl)-4(3H)-quinazolinone and {2-methyl-3-(2,4-dimethylphenyl)-4-quinazolone} and {2-methyl-3-(4-ethylphenyl)-4-quinazolone} still dreaming of analude xmas... cheers, toadie



		Antoncho (Official Hive Translator) 08-20-04 12:48 No 526463				Another interesting one
						Patent US3406173

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