OTC MDMA is now easy and cheap!!

[naturalblonde]

> 4)  Setup up the generator like you did for chlorine,
> and use the syringe to add NaOh and bubble ammonia into
> the methanol.  When all the lye has been added (might
> need to do 2 runs), pour in the bromosafrole, and seal
> tightly, VERY TIGHTLY.

Agent Smith, I totally like your OTC approach to life, even if it means sacrificing some yield. Good rules to live by.

No disrespect intended, but have any of your friends actually gotten the amination to work?

I don't fully understand the physical chemistry involved, but most chemical ammonia generators I've heard about don't really like to politely bubble NH3 into a solution in a closed system. Instead a backpressure seems to form and sucks the solution right back into the generator.

The ancient high-school colored-water/ammonia fountain is an example of this phenomenon.

Opinions? Ideas?

[Ghost_Of_BT]

The NH4 will bubble through methanol for a while before it starts sucking back. So just whip out the tube when it starts sucking.
Visit www.the-hive.ws

[Agent_Smith]

Suck back on the ammonia reaction is not as bad as some I've seen.  It can be a problem, check valves or such can help.  Personally I just whip the hose out like BT suggested.

Yes, it does work as described, I've posted yields.
blah blah blah something clever blah blah blah

[obituary]

forget the valve, take and find a way to get a plain glass funnel into your gassing chamber- yes, you might have to change the chamber your currently using to accomodate- anyway, run the hose in, attach the hose to the funnel and lower it into the solution by about a 1/4 inch, this will allow the gas to bubble through, but when the suckback occurs, it can only draw so much liquid before the the vacuum is broken, self regulating.  maybe not the most sophisticated of apparatus, but it does work.

[tomjuan]

So to recap your procedure, as well as add Rhodium's suggestion for making Br2, is this what we have?

halogenation
------------
Add sulfuric acid to sodium bromide (NaBr) to produce aqueous HBr acid
Add H2O2 to this mixture to produce Br2
Extract the Br2 with organic solvent like DCM
Add a small amount of iron to make some FeBr3 as a catalyst
Add naphthalene (mothballs) to the FeBr3/Br2 solution to produce gaseous HBr
Gas safrole to produce bromosafrole

animation
---------
Add NaOH solution to methylamine HCl to produce methylamine gas
Gas methanol to  produce methylamine/methanol solution
Add the bromosafrole to the methanol/methylamine
Seal the container, and shake occasionally for seven days.

extraction
----------
Do a full A/B extraction, recrystallization, etc...
-OR-
Acidify the rxn product to pH 2.
Filter out any solids
Evaporate the methanol away
Hope for the best as far as purity is concerned . . .

[Rhodium]

Make sure you separate all the DCM from the bromine before adding it to naphtalene/FeBr3, or you will perform a friedel-crafts alkylation/polymerization with the naphtalene.

[Osmium]

DCM is surprisingly inert in Friedel Crafts reactions, I´ve even used as a solvent for such reactions (with AlCl3 and acetyl chloride).

[Rhodium]

Have you? On what substrates? Both methyl chloride and chloroform is reactive in such conditions.

[tomjuan]

Would there be a less reactive solvent I could use for the Br2 extraction? Or is there a way to separate the Br2 and DCM without distillation? One good thing about this synthesis (if it could really be made to work with satisfactory yields) is that it doesn't require distillation or reduced pressure.

[Rhodium]

Diethyl ether should work.

[tomjuan]

Hmmm. Diethyl ether isn't exactly over-the-counter, although making it isn't that hard. Posts like this raise a little warning flag me. They might lead someone to believe they can just follow the indicated procedures and produce something safe and effective without knowing anything at all about the chemistry behind what they are doing.

I think I know someone who might try this synth in the next few days, and do a real write up on the results complete with yields and better physical descriptions of the appearances of the intermediate products.

[goiterjoe]

Diethyl ether is the stuff in starting fluid.  You shouldn't have any trouble finding it at the auto parts store. 
Drunk driving, that's what I like to do,
I like drunk driving with you.

[tomjuan]

The only types of starting fluid I can find around here have significant amounts of impurites, like heptane and ether-soluble lubricants. I have tried doing the water washing, but what I end up with doesn't even SMELL like ether. I certainly haven't given up on this route yet - I am still keeping my eyes open for new brands I haven't tried.

Regarding DCM, the separation of DCM (bp 39C) and bromine (bp 58C) is 19 degrees C. What would be the likely outcome of trying to evaporate away the DCM over a regular heat source without a column? Also, there was a claim that DCM wouldn't react and there might not be a need to separate the bromine after all - was there ever a verdict on this?

[b159510]

Regarding DCM, the separation of DCM (bp 39C) and bromine (bp 58C) is 19 degrees C. What would be the likely outcome of trying to evaporate away the DCM over a regular heat source without a column? I imagine the result would be incomplete separation. Br₂ rapidly evaporates at room temp where I live. A fractionating column should be used for volatile chemicals with a difference in bp less than 40°C.
Back to the Primitive

[Rhodium]

You can NOT evaporate away DCM from bromine, you would need to fractionally distill with good ventilation.

[tomjuan]

Yeah, that's what I figured - thanks for your answer.

[jacob019]

Is distillation the only way to get the safrole out of the sassafras?

[Osmium]

Freezing works too. UTFSE.

[jacob019]

How exactly would that work, does the safrole freeze and you just filter it out or does the other stuff freeze and your left with safrole.  What should the temp be taken to? And is isolating safrole realy necessary. Could you just use sassafras oil raw?  Sorry to be so inquisitive, but answers would make a good start for this recipe.  Thanks again.

[Osmium]

> does the safrole freeze and you just filter it out or
> does the other stuff freeze and your left with safrole.

The safrole will freeze first, it has a melting point of about 11°C when pure. 

> What should the temp be taken to?

Below the melting point of safrole. Freezer temps.

> And is isolating safrole realy necessary. Could you just
> use sassafras oil raw?

Depends on what synth you wanna perform, safrole content of your oil etc. It surely doesn't hurt to distill it.

> Sorry to be so inquisitive, but answers would make a good
> start for this recipe.

UTFSE. All this stuff has been talked about countless times in the past.