It was nothing special, really, just following LaBTop's procedure here:
https://www.thevespiary.org/rhodium/Rhodium/chemistry/redamin.nabh4.txt
.
750g store-bought MeAm.HCl (but it could have been made in one batch in a 5 liter RBF with AmmCl and formalin) were put into a container with a kilo of NaOH and shaken up some. A small cup of water was carefully placed in it and the lid with a hose with an inline valve was screwed on. The hose was attached to some coils of metal tubing submerged in a dry ice/acetone bath, and the other end of the tubing led to a flask also submerged in the bath. The gas generator was shaken up and the gaseous MeAm condensed into the flask with manipulation of the inline valve to prevent excess gas not being condensed, and also to prevent suckback between shakings of the generator.
When gas generation had mostly died down, the valve was shut and the receiving flask, which had been preweighed, was weighed again and showed about 305 g of MeAm had been condensed. 3 liters of MeOH was cooled in the dry ice/acetone bath, and the liquid MeAm was added to it. This was poured into a 20 liter flask (sorry, the 10 liter comment yesterday was a mistake. Swim was going to use a 10 liter jar but was having trouble getting a stirbar to spin on the slightly convex bottom. But 10 liters would be more than enough room.) situated in an ice bath on top of a magnetic stirrer, and 1000 beautiful grams of MDP-2-P was added. Approximately 300-400 g silica gel was added and it was stirred with a 2.5 inch egg shaped magnetic stirbar for 30 minutes.
The now orangeish solution was decanted away from the silica gel into a clean flask and the silica gel was rinsed with a small portion of methanol which was added to the other flask. The silical gel was removed from the 20 l flask and the methanol/imine was added back into it with the stirbar. The flask was placed back in the ice bath on the magnetic stirrer.
Stirring was started, and 100 grams of NaBH4 was added a spoonful at a time over the course of maybe 3 or 4 hours, making sure that the fizzing had died down and the temperature was below 15°C before each addition. After addition was complete, the mixture was allowed to stir for about 20 hrs.
The next day, most of the rxn mixture was poured into a 5 liter RBF equipped for distillation, and methanol was distilled off for awhile. When there was room, the rest of the rxn mixture was poured in and all of the methanol was distilled off. 3 liters of water was added to 1 liter of 31% HCl. This was poured into the 5 l flask and all of the residue dissolved. This was poured into a 10 liter jar and washed 2x with 1 liter of toluene. This was done by adding the toluene to the jar, shaking, letting the phases separate, pouring off as much toluene as possible, then pouring some of the mix into a 4 liter sep. funnel and separating, then pouring the rest into the sep. funnel and separating.
The aqueous solution was then basified with a sat. solution of NaOH to pH 14 and a golden brown oil separated out and fell to the bottom. The aqueous solution was poured away from the oil and the oil was poured into a beaker. There was still quite a bit of oil in the aqueous solution stuck to the sides of the glass, floating as beads, and such. DCM extraction was attempted but a big emulsion resulted so the whole thing was vacuum filtered through celite on a large buchner funnel. Some DCM was sucked into the pump, but oh well. The phases separated nicely after filtration and 3 extractions were done with 1 liter DCM each.
The DCM and oil were combined and washed twice with water and once with brine (1 liter each) using the technique of shaking in the 10 liter jar and separating in fractions in the 4 liter sep. funnel. The DCM was dried with MgSO4 (baked epsom salt), placed in a 5 l RBF, and the DCM was distilled off without vacuum to leave what looked like 750-800 ml of golded brown freebase oil. This was added to a 1 liter RBF situated in a heating mantle on top of a magnetic stirrer. The flask was equipped for distillation with a claised adaptor and a fractionating column (about 30 cm) packed with stainless steel wool obtained from a Chore Boy
TM scrub pad. Fast stirring was started, and heat and vacuum was applied. The vacuum quickly sucked the rest of the DCM into itself, so the heat was turned off while the pump oil was changed. Heat and vacuum was once again applied, and after awhile the temp quickly rose to 111°C (Swim isn't positive about this value, it's been awhile and he can't remember for sure but thinks this is what it was) with very few drops coming over before reaching this temp. The vacuum strength isn't known exactly, but is suspected to be somewhere around .4 mmHg because it pulls MDP-2-P over at a solid 100°C. Distillation continued at a rate of probably 2-3 drops per second for quite awhile and the temperature gradually dropped to 110°C due to the vacuum gradually increasing. Finally distillation slowed greatly and the temp started rising, so distillation was stopped. The preweighed receiving flask was weighed and the weight of water-white MDMA oil was 745 g.
This oil was added to 3 liters of ice cold anhydrous acetone and gassed with HCl and filtered repeatedly until no more precipitate formed. The crystals were washed with a small amount of acetone which was added to the gassed acetone and placed in the freezer. The crystals in the buchner funnel were dried by sucking air through them for awhile then by placing the whole mass on a piece of glass with a space heater blowing on it. Final weight was 793 grams of sparkly white MDMA.HCl. The next day there was quite a bit of precipitate in the acetone in the freezer. This was filtered, and cleaned up and the acetone was rotovapped down to about 600 ml and placed back in the freezer. More crystals precipitated.
After quite a bit of work to retrieve every last bit, Swim was left with 866 grams of clean, sparkly white MDMA.HCl.