palladium i use molar ratios and give examples in weight not ml
what you are looking at is a more concetrated solution of salts in the middle and a less conc. on the top.
add more water and swirl to mix the phases.
i also did tell you that you used too much sulfuric acid.
the ratio in moles
is
1 mole safrole/1.8 moles HBr
40% conc. in acetic acid by weight % denotes weight.

You cannot generate a substantial amount of the acid just by dissolving Br2 in water.
Wikipedia gives the reaction as:
Hydrobromic acid can be prepared in the laboratory via the reaction of Br2, SO2, and water.[2]
Br2 + SO2 + 2 H2O ? H2SO4 + 2 HBr
The SO2 is needed to reduce the Br2 into Br-

Actually Oerlikon, I think you have a mistake in that formula. that what I thought it was to but fractal corrected me:

H2SO4(aq) + 2NaBr(aq) = Na2SO4(s) + 2HBr(aq)

Unfortunately I used your formula resulting in me adding a 2x excess of H2SO4! Not good! I double checked all my calculations but forgot to check the equation. I think I might have messed this up completely now. I ended up separating the emmulsion and I dried the combined DCM extracts with MgSO4 or so I thought. when I tried to evaporate the DCM off on a warm water bath under vacuum I got two quite large layers and the color of the solution changed from an  opaque black to a light creamy brown colour. what the hell is going on? have I decomposed my product? I think I will start over with the correct ratios and watch out for emulsion and shit?

ill put up a few photos later of what's going on! weird.

Well, jon used that equatian and got it right!
Actualy he use 1:1 molar ratio of NaBr to H2SO4 with slight excess of NaBr
for reasons which akcom explained.

If that's only one layer that changed color in described manner upon rise of concetration
it's a good thing,you got brormo! (How does it smell!?)

Only you and God can know what othert layer might be,you added all sort of crap inside
while sepparating. What you added is what you got.
Take examples of both layer and test them for b.p.,smell,solubility,reactivity,pH...

Well,main reason why GAA is used instead of water as reaction media is that max. concentration
of HBr in water is too low to get enough bromosafrole.

You are basically suggesting to make HBr as gas and  dissolve it in GAA.
I thought that at first but it just isn't practical. Working with corrosive gases is
something you want to avoid at home at cost of adjusting every other parameter
of reaction to do w/o it! At least I do!

I don't get where is the problem,if it works don't fix it!

Adding a single Br at one side of the double bound (by the Markonikov's rule) that originates from ionic HBr
is MUCH more favourable than addition of the 2 Br across the double bound at both sides using neutral molecule of Br2 as source of Br.
Ratios seems to be adjusted just fine to do exactly that!
First you get most favourable reaction:
2 NaBr(s) + H2SO4(aq) => 2 HBr(aq) + Na2SO4 (aq)
Than you get two that are roughly equally favourable:
Getting bromosafrole and getting those unwanted redoxes.
Far least favourable one is one that concerns you:
-CH=CH2 + Br2 --> -CHBr-CBrH2
Not mentioning that concentration of reactant for this reaction
to happen (Br2) is effected by two previous reactions and it ain't favourable!

That is why you add the right amount of reactants that jon said,keep it cold
and don't let it react for more than one day.


 

what a good waste of safrole
that's why everybody is losing on this
mol seives, mgso4; i did'nt say any of that
just ftfd
follow the fucking directions!

You seem to be missing the point that Wizard is trying to make, it is broke and it needs fixed. Any concentration of H2SO4 above 74% has strong oxidising properties meaning its impossible to not make Br₂ with NaBr and H2SO4 without adding water. Acetic acid is not sufficient enough to assure that Bromine is not made.

If Br₂ is present you will get Dibromo safrole which will become a serious headache later on because it will aminate and it will also carry over with simular properties as MDMA. There is little mention of bromine becoming an issue quite possibly because the people that have performed the experiments are thinking that what they have is indeed MDMA when its not.

Well,main reason why GAA is used instead of water as reaction media is that max. concentration
of HBr in water is too low to get enough bromosafrole.

Not fully true, its used because the acid can act to catalyse placing OH across the double bound. This is the reason Mol sieves are used in these type of reactions that use (aq)HBr because its needed to remove the water and push the reaction to the right.

What Wizard is suggesting is by far the best way of generating insitu HBr for use in hydrobromination reactions. There is no Br2 formed, there is no gas formed since its insitu in an AcOH solvent and the concentration of HBr in Acetic acid is much larger then in water. Without water present there is also not the competing reaction of hydroxylation which can win out over bromination with ease.NaBr should be dissolved in AcOH and Phosphoric acid added because I highly doubt that Acetic acid is strong enough to push the equalibrium far enough to Hydrobromic acid. Concentrations of HBr in AcOH can be made as high as 70% IIRC.

I understood COMPLETELY what Wizard said but I think that dibromosafrole and coresponding diamine doesn't forma at all!
You don't get too much Br2,getting dibromosafrole is not as favourable as bromosafrole which consumes most of safrole from the start.

jon said it's O.K. and that he got MDMA and MDA many times using this reaction and I believe him. Not very scientific,I know...
Why would he lie!?

But!

If getting dibromosafrole and coresponding diamine is proved in this reaction Wizard is right!
What about substituting H2SO4 with H3PO4 and still keeping rest of the procedure!?

For those that aren't familiar with Uemura's posts from the Hve concerning the dibromide:

http://www.erowid.org/archive/rhodium/chemistry/mdp2p.dibromide.html

to describe Hive staff members as simply armchair chemists is rather humorous    Dr Strangelove was the first member of the Hive to get this method working, as was posted in the Grab your seats thread he used 48% HBr    As is often the case there's a rather interesting story behind that Hive thread from long ago, but that's for Dr Strangelove to tell if he cares to  

What about substituting H2SO4 with H3PO4 and still keeping rest of the procedure!?

Thats the point in the first place, Sulfuric is iffy, effective yet can lead to issues that could be avoided with a minor change in reagent nothing more.

Sedit: H2SO4's strength as an oxidizing agent is reduced in acetic acid.  This is basic inorganic chemistry.  I'm sure I have my old inorganic textbook laying around somewhere, but for comparison HOCl is a stronger acid in acetic acid if I'm not mistaken. Not only that, but we're not talking about 76% H2SO4, we're talking about 50% when its added to the AcOH.  On top of that, if the Br2 formation was so energetically favorable.

Anyway, the proof is in the pudding as the saying goes.  Jon has made it work.  I've yet to see anything other than arm chair speculation on the other side.

Because many people dont spout off failer anymore like was common place at the hive. There is a paper trail ten miles long of those claiming and I quote "I have wasted enough Safrole on this synthesis to fill a hot tub". No offense Jon and you should of all people see where im comming from that you should in no way shape or form take one persons advice on how to perform a reaction. You should study the mechanics, the patents, the failiars, and the success. After all of that try to find yourself in that place where you are 100% sure you can do it much better then the person before you.

You say that no Br2 is created in AcOH from this process then proceed to state that everyone is speaking from there armchair. Fair enough, go try it then. Add some NaBr to clean and clear GAA followed with a slow addition of H2SO4. Make sure to keep it very cold because I don't want this fucked up so that someone can say that heat is the variable to blame. After doing what I just asked you to please take a picture of this formed GAA/HBr solution and tell me what color it is.

Im positive at this point that the chair your sitting in is much more broken in then mine and has a nice ass print in it if you get my drift. Never accuse those of armchair chemistry when you dont know where they got there information from. From your point of view for all you know Jon is the armchair chemst and your just a sucker.... Not saying thats the case but if you never question it your acting foolish