Bright Star / Al/Hg/MeNH2 Questions

[Quicksilver]

I think I have this synth worked out to only 6 chems that you wouldn't find at your local hardware store (MeOH, MeNH2, p-Benzo, PdCl2, HgCl2, and DCM).  Any comments are always welcome.  Thanks. Neron:
1)What are you using methylamine for?  (MeNH2)  Did I misread, you do you mean nitromethane? (geez, now I feel like the Nitromethane Nazi... 

Post 196065

(Quicksilver: "Re: The Hive collaborative MDMA synthesis?", Methods Discourse) )

2)Consider modifying the protocol a-la Chromic/Osmium/psychokitty (and others) to use oxone.  And thus becoming slightly more otc. 
  

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxonemethod.txt

  

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxone.txt

[Neron]

My bad, SWIM meant MeNO2, not MeNH2.  Thanks for the info on the Oxone route, SWIM is gonna look into it quite a bit.

What do any bees think of a step-by-step, first timer's guide to MDMA?  SWIM thinks if he can practice this reaction a bit and come out with product at the end, it would help a lot of newbees out.  Maybe something like equipment descriptions and diagrams, reaction mechanisims, good directions and pictures for each step?  SWIM is going to make it as OTC as he can, so any suggestions are welcome.

[RoundBottom]

>What do any bees think of a step-by-step, first timer's guide to MDMA?

isn't that brightstar's all-in-one?  or methyl man's pair of Aces? (two Spades?!?  what kind of deck you dealing from, methyl?) 

[Neron]

Yeah, Bright Star's is a first time guide, but it's not as descriptive as some newbees would like (ok, that's an assumption).  It's kinda out of date, and you can do it with less reagents than he has specified.  DMF, p-Benzo, PdCl2, NH4Cl, and Paraformaldehyde are all not required (if SWIM can get this damn Oxone to work right).  We'll just have to see how good SWIM is at dreaming...

[RoundBottom]

how easy do we want to make this?  i do not think it should be as simple as shake'n'bake or instant cake mix.  it took SWIM about 1 year to go from lurking to first success.  and SWIM has about 350 pages of double sided printouts and research to learn from, and SWIM still does not know much more than the rudimentary mechanics of the reaction.

first, all these newly 'expert' bees flying around looking for reagents will definately muddy the water for the more cautious and discerning.

second, holding their hand will not guarantee they learn anything.  q.v. 'mokey see, monkey doo, monkey blow up garage.'

third, do we really need that much product out there?  well... i guess, maybe.

[goiterjoe]

the last few times SWIM distilled something, he noticed a dropoff in temperature between fractions due to nothing coming over.  he's never distilled a post-wacker slurry before, but it seems like it would be the same.  Do most of you notice a temperature rise in between fractions instead of a drop?

If pacman influenced us, we'd glide around dark rooms eating pills and listen to repetitive music.

[Neron]

Hmm... You're right.  SWIM is thinking about just making a mostly OTC route and do a write-up maybe ala Dr. Gonzo (photoessay).  SWIM was also gonna put in the reaction mechanism, such as describing what happens when liquid X is mixed with solution Y, etc.

[RoundBottom]

that's a great idea.  that would be the best safety net for newbees, to see as much as possible before, so they know what to expect.  once you've done a couple MM Al/Hg Amins, you've pretty much got it down (as long as it yields). 

probably showing each wash and extraction, and what to expect, then what part to keep would be the best assist.

[Neron]

SWIM'll get working on that   .  SWIM also has another question; can any Hg salt work in place of HgCl2, such as HgSO4?  SWIM noticed how easy it was to make (Hg + H2SO4) and thought this would go well with the OTC method, seeing as how one would only have to acquire a small amount of mercury and some drain cleaner.

[Chromic]

GJ, I see that happen when distilling anything that is high BP with a column. I think it's because the top of the glass is cooling down rapidly while the distilling flask is heating up to boil off the next fraction. I also think it's a good indication that I need better insulation around my flask / column / 3-way, or to get a better vacuum.

[goiterjoe]

it happens because the liquid that boils hits the thermometer as it is going through the 3-way adapter, and when that fraction is done, the air in the condensor and receiving flask, which is much cooler, draws back over and surrounds the thermometer while the next fraction become hot enough to boil through the column.  I would imagine that you have to use a column to distill out the post wacker, but maybe I'm wrong.


If pacman influenced us, we'd glide around dark rooms eating pills and listen to repetitive music.

[cosmicwater]

Why would you separate from the undistilled products...why not just add appropriate amounts of reactants again to liquid PdCl2 and re-react?  Catalyst by definition is not consumed in reaction so recycle should be possible and at KB prices, I'd personally try to recycle somehow.  2c
I will be trying this shortly and let you know if it works.