First, helional is oxidised to helionic acid:
http://bbzzzsvqcrqtki6umym6itiixfhn...of-mda-from-helional-report.17878/post-103234
Then the Hunsdiecker reaction is carried out. For this reaction, I decided to first try using potassium salts, as this reaction works with salts other than silver salts.
1 g of helionic acid is placed in 10 mL of water containing 0.27 g of KOH. Stirring is activated and the solution is evaporated at 110°C. The salt is thoroughly dried, as water is detrimental to the reaction. The salt is placed in 10 mL of EtOAc, but not all of it dissolves. Stirring is activated and the solution is heated to 50°C. Then Br2 (1.2eq) formed with HBr and H2O2 is added and gas is immediately visible (probably CO2). The mixture is left at this temperature for 10 minutes, then water containing NaHCO₃ and a few grains of thiosulphate is added, and EtOAc is extracted and washed with water, dried with NaSO₄ and EtOAc is evaporated. A very viscous oil is obtained when cold. By replacing Br₂ with I₂, a partially crystallised oil is obtained after 2 hours. TLC shows that a reaction has taken place, with an Rf spot of 0.345 in the 80:20 heptane:EtOAc eluent.
I don't have time to study this reaction further, but I would like to hear feedback from people who have done it or want to do it, because I think it is easily scalable and would be a good way to make MDA or MDMA. I also haven't had time to characterise the product obtained, but it seems to react with MeNH2 or NH3, because the spot disappears by TLC. Eventually, I will try to optimise this reaction and make sure it works. It would also be necessary to try silver salts to see if they give better yields, and to try different solvents.
