Where did he say that, and which alcohol did he refer to?
https://www.thevespiary.org/rhodium/Rhodium/chemistry/ritter-alhg.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/ritter-alhg.html)
"Mix up about 1.5 or 2 liters of 35% NaOH solution and allow to cool. Slowly add the gray aluminum gook produced in the first reaction to the NaOH solution and pour into a large separatory funnel. Two distinct layers will appear after sitting for maybe an hour, the top being a reddish alcoholic solution of product and the bottom garbage NaOH/Al(OH)3. Simply separate off the garbage bottom layer and discard. Don’t worry, there’s no product tied up in it...
Didn't you dump that layer? And if you suggest to extract alcohol with xylene, I'm not sure that will work good, add lots of water or even better - evaporate most alcohol under vacuum.
Yup,didn't notice that mistake.It should have read "add xylene to alcohol layer and add some water.
I'm not sure that will work good
In raf experience it does,alcohol and water form their own layer.
How do you suggest to isolate the MDMA.HCl from this alcoholic solution? If you are just going to evaporate it, then you need to recrystalize it before you are done to remove impurities.
Raf thinks distillation and following acetone wash removes most of em.Raf will probably try gassing or titrating freebase in acetone.With impure freebase gassing was difficult as it oiled out,maybe with purer freebase it works.
Most definitely extract 1-2 times with xylene here, then dry the solution over magnesium sulfate or equivalent before distilling
Why dry?BP difference between water and freebase is nearly 200 C,i don't think it will interfere with distillation procedure.
First, Ritter is referring to the solid grey sludge not holding any product, any water/alcohol above it should be processed.
In raf experience it does,alcohol and water form their own layer.
But you did not mention any water added, just alcohol (and you didn't specify *which* alcohol).
Raf thinks distillation and following acetone wash removes most of em.
Yes, but new ones form as you are treating the freebase with acid, just watch the colors - if it isn't water-white and clear, you have impurities which should be removed. Take pride in the purest possible product!
With impure freebase gassing was difficult as it oiled out,maybe with purer freebase it works.
Most certainly, make sure you have dry solvents and use 10x the volume of solvent to freebase (madmax has written good posts on this).
Why dry?BP difference between water and freebase is nearly 200 C,i don't think it will interfere with distillation procedure.
Post 439125 (https://www.thevespiary.org/talk/index.php?topic=10433.msg43912500#msg43912500)
(hypo: "because water sucks", Newbee Forum)
pH 14 at room temp for short periods is okay if necessary, but you WILL see decomposition if you heat it (as in trying to boil off any alcohol), red tars forming and your yield drops like a countdown timer...
I'd say that pH 11 is always safe with our most common compounds, but I wouldn't be scared of pH 12 either - but why go higher than required for the MDMA to become a freebase and/or the Al/Hg reaction running at a reasonable speed (as in a gentle reflux at most, forced wild boiling is unnecessary and stupid).
1) The end reaction should be basic in a standard MM Al/Hg?
Yes, It's basic as is, because of the rxn: Al + 3 H2O => Al3+ + 3 OH- + 3 H2
2) The added base is to help separate the layers and reduce the "aluminum crud" in the solution?
Yes, to decompose all traces of residual Al metal, to turn any formed Al2O3 to Al(OH)3 (more granular, easier to filter) and increasing the ionic strength of the aqueous solution (making the alcohol separate).
Therefore - Bee's should only add as much NaOH solution as needed to separate layers in workup?
Yes, pretty much so in my opinion. There are a lot of people doing other things, but their strategy is more based on a desire to skip steps and take short-cuts than to increase the purity and yield of the product.
The MDMA is already an oil so the NaOH is not doing anything to the product we want, just adjusting other things in the solution?
Yes, exactly. Addition of more than 2 mL of 25% NaOH to the reaction mixture for every gram MDP2P you begun with is really unnecessary.
The Al/Hg procedures on my page for making Meth from P2P (https://www.thevespiary.org/rhodium/Rhodium/chemistry/p2p-meth.html)
(https://www.thevespiary.org/rhodium/Rhodium/chemistry/p2p-meth.html) are identical to what would be used if making MDMA, just use 1.35 times the weight of MDP2P than P2P in those examples (to compensate for the higher molecular weight of MDP2P) - other than that change nothing. Note that the procedures differ pretty much when it comes to small details, but all the important things are kept the same - illustrating that you can be flexible in SOME places, but not in others, you need to know what is critical or not.