Tramadol (Ultram) synthesis

[Plinius]

Hi everyone,

After most than 8 attempts, I didn’t succeed to produce Tramadol, at least, no more than 5mg but probably other molecule.

Know, my Grignard reaction is correct, the temperature to ignite 3-Bromoanisol+Mg flakes seems to be 70°C +/-2°C under constant agitation (the agitation is important to scratch the Mg surface and remove the oxide. At least in one good point.

Then I think my problem come from Mannich synthesis : my product DON’T crystalize in acetone : crystals are forming a denser liquid phase automatically.
I remove 95 % of the acetone and make the denser liquid phase evaporate on 60°C plate, to harvest white crystals.

But then, if I try to recrystallize them again from acetone, the same way, the product lose 70 % of weight and keep same properties.

As the 2-dimethylaminomethyl-cyclohexanone hydrochloride should melt near 157-158°C, I assume they are not the Mannich.HCl expected right ?

Does anyone can give me some tip ? Or better, try himself and share his result please ?

(here, a picture of « fake » Mannich.HCl crude 10mmol, before recrystallization.)

 

[G.Patton]

Do you use pure dry acetone? Hi, sorry for a long reply. I haven't seen your question.

 

[mefistofeles]

im sure it has to be anhydrous acetone

 

[IHeisenberg]

I’m having trouble with grignard
Now I practically react 2-dimethyl aminomethyl cyclohexanone with Grignard reagent and I see temperature rises with every drop of the free base but when I quench the reaction with ammonium chloride I see small temperature rises with only few drops .
After distillation of the solvent and adding acid ( hydrochloric acid ) the product didn’t crystallize.
Maybe some moisture get contacted with the reaction because the apparatus may not well sealed.
Can this moisture breakdown the reaction Before quenching.

 

[G.Patton]

Why did you quenched the reaction with NH4Cl?

 

[IHeisenberg]

Remind

 

[G.Patton]

Please, don't spam like this. It's worth to write me in DM instead.