MDMA old skool

[chem_123]

It's bee-n a while for SWIM, SWIM'd appreciate some feedback (good or bad):

Is it logical if SWIM has limited access to chemicals from a lab to follow the following guidelines (with success?, is there a lot of sacrifice on yield because of the chosen route?):

- safrole from sass. oil

- isosafrole from safrole reflux with KOH pellets (can NaOH powder bee used?)

- MDP2P from isosafrole using oxone method by chromic

- MDMA from MDP2P by using the Al/Hg/Nitromethane route by Methyl Man?

- MDMA.hcl from MDMA using hcl gas or the xylene/ipa method

[Rhodium]

NaOH has been used too with success, UTFSE for details (search for "naoh isomerization" or similar).

Chromic's Oxone oxidation is okay, but also take a look at

Chromic's Peracetic Acid Oxidation

(https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html)

- MDMA from MDP2P by using the Al/Hg/Nitromethane route by Methyl Man?

Do not follow that version verbatim as he skips a lot of essential purification steps in the end - perform a proper acid/base extraction after the reductive amination, and please distill the freebase before crystallizing it.

- MDMA.hcl from MDMA using hcl gas or the xylene/ipa method

Definitely gas the freebase in toluene, ether or similar. Some claims that even acetone will work. Then, as the final step, perform a proper recrystallization of the salt, as described in

Post 454897

(Rhodium: "Recrystallization of MDMA.HCl for Purity", Methods Discourse)

[chem_123]

Chromic's Oxone oxidation is okay, but also take a look at Chromic's Peracetic Acid Oxidation (

https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracetic.chromic.html

)

SWIM's instantly fallen in love with Chromics peracetic method, tyvm Rhodium, and ty for the other two tips  

Something SWIM neglected to mention...there is the question of using mercury iodide[sic]? as a substitute for HgCl2 in the Al/Hg  reductive amination...

and about the osmiums al/hg varioation...good over MM?

[Chromic]

Oxone is great if you can't get acetic acid and hydrogen peroxide (but who can't get these chems?)... the results at making ketone weren't great. Others have posted better success--but using Oxone is risky as the purity isn't always known. I'd honestly prefer to use vinegar, baking soda and sulfuric acid to make the GAA if you can't get pure GAA over using oxone... plus making GAA at home is a good intro to making the other chems. It's a good learning experience IMHO. Then again, you must remember I'm an OTC bee.

Hydrogen peroxide is easily available, so is GAA so it shouldn't be too hard to source either...

KOH is also really easy to source... no reason to use NaOH, but it does work too.

[nitrous351]

SWIN will tell you that his virgin run was the exact thing you posted. Yields from 100g of olefin was 12 grams of salt. I heard it was really good though. SWIN told me it was so good because he followed rhod's advice and distilled everything, and recrystalized at the end.
Now, SWIN does the peracetic method with the MM Al/Hg. SWIN says the yields are much better now. Maybe you should try the peracetic with a Os/BS Al/Hg. SWIN's been reading up on it lately, and it doesn't look too difficult to pull off (plus it sounds a lot gentler than the MM version).

[chem_123]

There is nothing but contraversy towards the crystallization step.  SWIM just finished reading a document where all the users must have been on something...D.A.'s method of...

Light Golden MDMA freebase was dissolved in ~6x it’s volume of acetone.  It was found that making the solution more dilute than the old 1:4 was very beneficial because crystallization can occur without any cooling.  The flask was placed in an icebath on top of a stirrer and the solution was allowed to rapidly stir and cool down.  Next, conc. Aq. HCl was slowly pippetted (really fast dripping) in repeatedly and the pH was checked with water wetted pH strips until the pH was 2-4.  about a third of the way through the addition of HCl, the solution will have exploded with granular crystals (like NaCl as opposed to fishscales from DCM crystallization).  The flask is covered and placed in the freezer overnight and the next morning, the solution is filtered to recover ~90=96% of the product.  If the product oil was dirty then washing with a bit of ice cold acetone will clean and lighten it up.  Evaporate down the mother liquor, re-dissolve in 1/3 the original amount of acetone and throw back in the freezer to recover the final bit of product.

...does it produce the right result...nice white MDMA.hcl crystals?

[nitrous351]

toluene (make sure you dry it first) if you can get it. If you can't get toluene, xylene (make sure you dry it first) works fine too. SWIN hasn't tried any other solvents for crystalization, so he can't offer any advice about anything else...
SWIN's not too sure about this, because he's never titrated before, but sounds like DA is adding too much acid. SWIN's pretty sure he remembers that a pH of 4-5 is sufficient to get crystals. Of course, it would bee safe to have a titration-experienced bee to confirm/deny this statement. Or why doesn't SWIY try gassing with HCl instead? The result is more powdery product. With titrating or gassing, SWIY should get snow-white crystals, but it's ALWAYS good practice to wash them with ice-cold acetone. Sometimes, if you overgas or overtitrate, SWIY will get tannish or pinkish colored crystals, but the ice-cold acetone wash should whiten them up. After the ice-cold acetone wash, it's always a splendid idea to recrystalize using a minimum volume of IPA. Also, when SWIY recrystalizes, the slower he lets the IPA cool down, the purer the product will bee. The result will make SWIY cry tears of joy! good luck

[doktor_alternate]

toluene and water form a low-boiling azotrope, so drying toluene is a simple as distilling it.