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.thevespiary.org/rhodium/Rhodium/chemistry/quaalude.html
.
And the analogue is described here:
Patent US3162634
.