Hello everyone, as a lot people recently ask me to help them via this synthesis i decided to write one fast and good recipe for this exact compound.
1st. We are gona prepare the building block for this beloved cathinone, its isohexanophenone, this is easily and cheap synthesied by FC alkylation.
Chemicals needed :
Isohexanoyl chloride, benzene, dce, alcl3 or other lewis acid.
Procedure :
Firstly prepare your lewis acid complex with your substitued benzene derivate, by mixing equimolar amaunts of the two reagents into the reaction flask, and drip the equimolar amaunt of isohenoyl chloride.
Add X amaunt benzene to the flask, aply cooling and add Z amaunt alcl3, stir and add carefuly the Y amaunt of acyl chloride, (HCL gass produced as byproduct !!! )
Afther the all isohexanoyl chloride is added, remove the cooling and heat to 30C for 2,5h, then remove from heat, prepare an ice bucket with hcl acid and pour the reaction mixture into it. The ketone and solvent will get on top usualy. Put the top leyer into the separetory funnel and wash good with sodium carbonate solution, destill of the dce with rotovap, then fractionate your ketone to obtain it clean. Yield of the procedure araund 70% and even better if performed with care !!!
Step 2. Halogenation of the purified ketone. (A-bromo-isohexanophenone).
I will recomend to use N-bromosuccinimide for this work.
Now put your purified ketone into the flask, add 1/10 molar mass p-TSA, equimolar amaunt of NBS, and GAA acid as solvent and reflux until all succinimidine is precipitated into the flask and reaction is ready. Filter off the liquid, destroy the acid with sodium carbonate and extract the bromo-ketone via sepration funel. (Its liquid)
Step 3. Pour the a-bromo-isohexanophenone into the reaction flask, add a little bit potasium carbonate (catalyc amaunts) , use Ethyl Acetate as solvent, and drip the pyrrolidine into the flask with stiring and cooling, afther all pyrolidine is added, stir until all ketone is transformed control via TLC or just let it stirr for 12h. Afther reaction is completed, pour the reaction mixture into the sepratory funnel and add brine solution to wash the exessive pyrrolidine, then again remove the Ethyl Acetate by destilation in rotovap and even the a-pyrrolidino-isohexanophenone freebase is stable to be destiled if needed. Then mix the freebase with cold acetone and gass with HCL acid. The yield is very high for all the procedures. This results into reacemic powder, for crystals seperate isomers and crystalize them seperatly.
Good luck haha
1st. We are gona prepare the building block for this beloved cathinone, its isohexanophenone, this is easily and cheap synthesied by FC alkylation.
Chemicals needed :
Isohexanoyl chloride, benzene, dce, alcl3 or other lewis acid.
Procedure :
Firstly prepare your lewis acid complex with your substitued benzene derivate, by mixing equimolar amaunts of the two reagents into the reaction flask, and drip the equimolar amaunt of isohenoyl chloride.
Add X amaunt benzene to the flask, aply cooling and add Z amaunt alcl3, stir and add carefuly the Y amaunt of acyl chloride, (HCL gass produced as byproduct !!! )
Afther the all isohexanoyl chloride is added, remove the cooling and heat to 30C for 2,5h, then remove from heat, prepare an ice bucket with hcl acid and pour the reaction mixture into it. The ketone and solvent will get on top usualy. Put the top leyer into the separetory funnel and wash good with sodium carbonate solution, destill of the dce with rotovap, then fractionate your ketone to obtain it clean. Yield of the procedure araund 70% and even better if performed with care !!!
Step 2. Halogenation of the purified ketone. (A-bromo-isohexanophenone).
I will recomend to use N-bromosuccinimide for this work.
Now put your purified ketone into the flask, add 1/10 molar mass p-TSA, equimolar amaunt of NBS, and GAA acid as solvent and reflux until all succinimidine is precipitated into the flask and reaction is ready. Filter off the liquid, destroy the acid with sodium carbonate and extract the bromo-ketone via sepration funel. (Its liquid)
Step 3. Pour the a-bromo-isohexanophenone into the reaction flask, add a little bit potasium carbonate (catalyc amaunts) , use Ethyl Acetate as solvent, and drip the pyrrolidine into the flask with stiring and cooling, afther all pyrolidine is added, stir until all ketone is transformed control via TLC or just let it stirr for 12h. Afther reaction is completed, pour the reaction mixture into the sepratory funnel and add brine solution to wash the exessive pyrrolidine, then again remove the Ethyl Acetate by destilation in rotovap and even the a-pyrrolidino-isohexanophenone freebase is stable to be destiled if needed. Then mix the freebase with cold acetone and gass with HCL acid. The yield is very high for all the procedures. This results into reacemic powder, for crystals seperate isomers and crystalize them seperatly.
Good luck haha