::beats head against wall:: NO GODDAMNIT.. CHCl3 or DMF, read the %@#$^%@#$ post!

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blah blah blah something clever blah blah blah, email at dateline@nbc.com

about this: it seems as though the moth balls turn the bromine solution into a gas that then bubbles into the safrole, right??
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Brominating Safrole

1) Empty your Cl2 gas generator and clean it out.

2) Pop the bromine/catalyst solution into the bottle.

3) Get some old fashioned mothballs. You'll notice that they are nearly 100% naphthalene: perfect, an ideal aromatic. Crush about 100grams of mothballs, not too fine though, leave it chunky. You're going to add this is two additions, so divide it in half.

4) Take the long tube from the gas generator and put it into a bottle of 30gs of COLD safrole. Run the tube through a cold water bath before it reaches the safrole, this will cut down on how much bromine is released (It's not really a prob. but bromine is a volitile liquid). It'd be ideal to have a bromine trap chmaber, but it is optional. The ~30gram bottles of sassfrass work great as a container to brominate in. Plug up the short tube, you're not going to use it.

5) Throw in one half of the crushed mothballs and quickly seal the gas generator. When the reaction stops completely, add the rest of the mothballs and seal again.

I'll answer this question: yes, you're correct just as the post says. Bromine+Napthalene+lewis acid->Hbr(g).
I would chill(-13)the bromine solution and keep it in ice bath during the hbr production.that should help keep the bromine under control. as well as using a drying tube(or small jar filled with crushed damprid/calcium chloride) before the gas hits the safrole which idealy should also be in ice bath for maximum yields.

Why are you folks torturing yourselves trying to produce anhydrous HBr. The DMSO method really works!

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  The christian god hates your soul. Care for a little necrophilia?

Nope.  At leats not for me, or the majority of bees.  I suppose it does work in theory, however the DMSO does nothing to prevent cleavage which is the major problem in this area.  In fact as I've said hundreds of times those DMSO color changes indicate everything is going to shit.  Fuck, what do u think is going to happen if you sit safrole with H2SO4 for a few days?!

Granted that everyone gets color changes in DMSO, that means everyone is getting cleavage.  That means that in order to make it work you need to establish a careful balance between the rate of cleavage, and the rate of bromination.  So far no one has given a reliable set of guidelines for temperature, length, ratios etc.  As such, this is still a more robust method, depsite its comparative complexity.

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blah blah blah something clever blah blah blah, email at dateline@nbc.com

"Fuck, what do u think is going to happen if you sit safrole with H2SO4 for a few days?!"

  Just make sure that you use excess Na-bromide and you won't have to worry. After mixing the bromide/H2SO4, let it sit for 24 hours to make sure all sulfuric acid is neutralized, then add your allylbenzene. Pugsley isn't full of shit.

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  The christian god hates your soul. Care for a little necrophilia?

The problem is that noone has ever analyzed the composition of the post-reaction "bromosafrole". And I don't think anyone distills it afterwards even, to get an approximate yield determination. According to forensic journals I have in my offline paper archive, the 1-bromo, 3-bromo and 2,3-dibromo compounds are all side products in the reaction, as well as some stuff with a destroyed MD bridge.

Could someone PLEASE distill the formed bromosafrole in any reaction, and then post the yield of stuff coming over at the right temperature (of course after a dilute base wash to remove phenols).

I wish I had only half the safrole wasted on this procedure in the last ten years, I probably could fill my big ass party jacuzzi with it.

How's this for an idea: Add phthalic or acetic anhydride to a solution of acetic acid, 48% hydrobromic acid, and safrole?

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  The christian god hates your soul. Care for a little necrophilia?

That would be an idea. Please tell us how it works out.

Could the bromosafrole? be tested by dropping it into cold H2SO4, and hoping it don't dissolve, or is there some other reliable method. Btw, it can't involve distillation, because my vac-pump was cooked by formic acid.
  There is a very reliable way to produce anhydrous HBr, but it might not be for everyone, because I'm guessing that lithium bromide's expensive? Anyway, here's a piece of a patent that gave me a chubby:

US3199953
Process For Production Of Anhydrous Hydrogen Bromide From Lithium Bromide

  Into a turbomixer having approximately a 100ml capacity was charged 61g benzoic acid and 15g (approximately 0.15M) of lithium bromide. The mixture was heated to a temperature in the range 250-260*C with stirring, and nitrogen or carbon dioxide gas at a flow rate of 235ml per minute was passed through the heated mixture. After 1 hour at temperature, approximately 80% of the theoretical amount of hydrogen bromide had been evolved. At 2 hours, 89% of the theoretical hydrogen bromide had been evolved. The reaction is substantially complete after 4 hours of reaction time.
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  In this reaction, would the lithium bromide be converted to lithium benzoate? How would one go about extracting and re-forming the bromide? Peace!

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  The christian god hates your soul. Care for a little necrophilia?

In the lab Br2 is ususlly made by heating NaBr with MnO2 and sulfuric acid.

I guess the red P stands in the way of the simple lab prep of HBr from dripping bromine on  RP and H2O mixed with a little sand to slow the rxn. A u-tube with RP dries the gas and removes residual Br2.
  As much as I love industrial chem, I got bromine on me once, and to this day hate the stuff.
  The comment on not being a chem mjr, till p-chem was right, that's a hard fuckin course, and I used to be a physics major, though I came to love both HOMO and his retarded cousin, LUMO.

I doesnt seem to have been brought since my last post - KBr is no longer OTC in my area - 2 Home Depots that had it dont no more, all replaced (not simply out of season) with much more complicated sounded chems!

Also - could someone estimate amount of Br2 produced by 1 lb of 98% KBr? Is that enopugh for 50 ml Br2?

you should theoretically obtain about 223ml Br2 (density ~3g/ml)
per kilo of KBr

Karl, 223*3 = 669 gr > 1 pound. Check your maths.

SI units are cool

Just to specify the name of the quat sufactant named early, early on in the post. It is Arquad-C50
(n-Alkyltrimethylammonium chloride) from bounce drier sheets.

hello, i'm new around here, I'm from Brazil. I really apreciated your work to turn an completely OTC MDMA synth true.
I've read somewhere around this topic, that there is an easy way of making ammonium sulphate from the Home diluted Ammonia that can be bought in any pharmacy, and would turn this synth more OTC...COuld anybody here tell me this way??
And one more thing... Where should I look for NaBr????And what is his OTC use....
Thanx!!!!!!

Reacting ammonia with an acid makes an ammonium salt. E.G.
React NH3 + H2SO4 --> ammonium sulfate

I just read through this thread and I dont understand how it could work. First he starts off with sassasfras oil and doesnt distill anything? And he gets 30% yields from sassasfras, thats crazy. I myself dont believe this procedure.