Alright from trying the procedure a few times over, getting varied results.
Ive tabulated my previous experiments and I ended up with this.
Im getting a pretty even yield using this:
20grams piperonal,17ml nitroethane, 6.4g ammonium acetate anhydrous, in 45ml GAA. This is stir at room temp until everything is dissolved and once a slight discoloring observed, it is set up for a gentle reflux for two hours. Solution is a dark red/brown. This is left to cool to room temperature and is then poured into 1500ml dh20 with enough ice to just cover the surface with stirring (total time ends around the 3h mark). Yellow chunks precipitate. I receive an average of 23 grams from this, about 17-18g after recrystallizing with methanol. From that I've been using the mercury/aluminium amalgam to reduce the nitropropene. Every batch where the reduction hasn't worked its always been when I have used thick tin foil, and I would end up with much of it unused. I now use Reynolds thin tin foil. Its allot to shove down the neck of your flask mid reaction though. but hustle through that shit! gloves, goggles and respirators! I aim for my reduction to be finished by the second hour. I've only ever had to use a damp towel once, and that was out of carelessness. Anyway, two liter flask, and a leibig condenser, and a nice chunky stir bar (I use a 70mm bar and don't ever really have a problem here).
I used 200ml GAA, 350ml methanol, 15gram nitroproene and an extra 30ml to wash the beaker and the funnel after the solution has been poured into the flask. 0.75g mercuric chloride dissolved in 20ml hot water. 35g foil, cut into small squares (2cm x 2cm) and lightly blenderized. I have never tried pre-amalgamating the foil, I don't know if this would increase yields perhaps? I've only ever had the reaction peter out upon addition of thick foil. after-which I basify it strongly, slowly, and with moderate cooling, with a 750ml ice cold solution of 35% NaOH. I then extract with 1000ml toluene, distill this off until an oil remains. I dissolve this in a 5% HCl solution. Aqueous layer turns skin-peach. Some undissolved crap at the bottom is dissolved and removed with 100ml DCM, as a deep red brown layer. solution is basified again, and again extracted I personally use toluene here. dry it over calcium chloride, leaving a clear lager colored solvent, which is then gassed. Yields me about 6g of white/off-white MDA HCl consistently. mp is only ever within 10 degrees of the stated mp of 185c.
What am I overlooking or doing wrong?
And what is the consensus on al powder? too fine? could this be made into an amalgam slurry that could slowly be added into the reaction mix, at a slow enough pace, or is it just totally going to get away from me and paint the ceiling?
got some rad photos too.