following Antibody2's acidic al/hg reduction of the mdp2p oxime to MDA follows some type of curve where a higher ratio of Al leads to MDA whereas a lower ratio of Al leads to MDOH. this leaves me with 2 questions
1.
why does the amount of Al affect the ratio of MDOH to MDA produced?
2.
also, in his writeup he adds Al periodically throughout the reaction. you'd think if you don't time the addition of the Al correctly then you risk more MDOH formation. you'd think a better way to go about this is add the MDP2P oxime incrementally like other Al/Hg's. Chromic adds all the Al at once at the beginning, waits for the amalgamation then adds the MDP2P oxime all at once along with the AcOH. I think this sounds like a better way to go about it because the time period in which additions are performed depends on the scale of the Al/Hg. Smaller Al/Hg's run faster of course and larger runs run longer. So I like Chromic's variation a little better as to avoid MDOH formation by potentially adding the Al a little too late which would cause MDOH formation one would think. The only thing is that Chromic ran it on a small scale using only 6.4g MDP2P oxime and he said it ran hot and fast with an impressive MeOH reflux (Chromic used MeOH instead of EtOH) but quickly petered out. If it were scaled up x4 then one would worry about a runaway reaction of adding all the MDP2P oxime at once. It's definitely one of those things you just have to run a few times and get the hang of the reaction to be able to know the best addition route.
Antibody2's original write-up:
h**p://www.erowid.org/archive/rhodium/chemistry/alhg.oxime.html
here is Chromic's variation:
here's a run Antibody2 did that focused on MDOH instead of MDA:
1.
why does the amount of Al affect the ratio of MDOH to MDA produced?
2.
also, in his writeup he adds Al periodically throughout the reaction. you'd think if you don't time the addition of the Al correctly then you risk more MDOH formation. you'd think a better way to go about this is add the MDP2P oxime incrementally like other Al/Hg's. Chromic adds all the Al at once at the beginning, waits for the amalgamation then adds the MDP2P oxime all at once along with the AcOH. I think this sounds like a better way to go about it because the time period in which additions are performed depends on the scale of the Al/Hg. Smaller Al/Hg's run faster of course and larger runs run longer. So I like Chromic's variation a little better as to avoid MDOH formation by potentially adding the Al a little too late which would cause MDOH formation one would think. The only thing is that Chromic ran it on a small scale using only 6.4g MDP2P oxime and he said it ran hot and fast with an impressive MeOH reflux (Chromic used MeOH instead of EtOH) but quickly petered out. If it were scaled up x4 then one would worry about a runaway reaction of adding all the MDP2P oxime at once. It's definitely one of those things you just have to run a few times and get the hang of the reaction to be able to know the best addition route.
Antibody2's original write-up:
h**p://www.erowid.org/archive/rhodium/chemistry/alhg.oxime.html
here is Chromic's variation:
Quote
I watched the crazy old man with the dark trimmed glasses go at it again. This time he fucking amazed me! I saw him do something like 125ml MeOH, 25mL H2O, pinch HgCl2 (i'd say about 50mg or so), stirred. 8.9g Al, stirred ~20 mins. Added 6.4g isosafrole ketoxime, added 25g HOAc. ~3 hours pass with mag stirring (flask is only warm to the touch). Slowly added 90g NaOH dissolved in 200mL ice-water. Extracted with 80ml, then 45ml toluene. Washed with 150ml 5% NaOH, filter, 150ml 5% NaOH, 150ml brine. Titrated to pH 4 with HCl in distilled water with stirring. Evaporated water. 5.9g MDA.HCl yield (before recrystallization). (83% crude yield!!!)
The reaction ran HOT and FAST. It was over and done in about two or three hours. The yields are FUCKING STELLAR.
Antibody gets two thumbs up for this procedure!!!
Things learned (this is his third run of ketoxime reduction, btw):
1) you can use MeOH instead of EtOH, which is good news
2) you can amalgamate all the Al before hand and in situ as MM does (very good news!)
This definitely paves the way for OTC MDA.HCl in high yields! (or is it really MDOH.HCl? ahh, who really cares!)
HAPPY, HAPPY, JOY, JOY!!!!!
reaction ran hot during the first hour, with a healthly reflux, then petered out quickly. It was over by two hours and was warm to the touch by the third hour. 83% yield is the highest yield I've ever gotten with an Al/Hg. I can't believe it happened with a ketoxime reduction... The MDA/MDMA mixture is phenomenal! it was 75mg/75mg... it included dreaming while awake, long-lasting buzz, full pupil dilation, intense euphoria... all round it's highly recommended!
here's a run Antibody2 did that focused on MDOH instead of MDA:
Quote
Antibody2:
A recent batch of MDOH was prepared via Al/Hg redxn of the ketoxime using 5 equivalents of Al and HOAc, 150mls H2O, 200mls IPA and 1650mls MeOH using the above proceedure. (10x produces higher yeilds with a much higher MDA ratio) In an attempt to further isolate the MDOH, its lower solubility in alcohols was exploited, and was slowly recrystalized from an equivalent w/w of boiling MeOH. The crop of crystals that formed when the solution had cooled to RT were vacuum filtered. The balance refridgerated to produce a second crop. Then reduced and and refridgerated to yield a third. (yeild ca. 72% w/w from oxime)
The odour of the first and to a large extent the second crop was completely dissimilar to MDA. The odor could be characterized as sweet. If you are familiar with MDA there is no mistaking the two.
Only time I was able to recover what I suppose is the oxime, is when I didn't add any water post-reaction. Then I putted the reaction content in the freezer, but only for 35minutes, then suction filtered and washed it with cold water, but It again turned back to the ketone. Was able to recover a whole 300mg of what I supposed is the oxime. Only way I can test now is with marquis reagent and it actually turns purple after drying.
?
The work up using methanol as a solvent is more difficult because of the sodium acetate that's produced during the reaction so it's better to use EtOH or IPA 
One can use sodium borohydride with titanium tetrachloride or nickel Chloride as well 
These reductions can be done using THF as a solvent too 
It's certainly possible to get the ketone from the oxime, that's one of the ways that p2p is made 