#1  I didn't calculate the stoichimetric ratios.  I stole that bit from Iudekx, I know it works, but stoichiometricly it might very well be wrong.  Balance equations and finding molecular weights is so boring....

#2  Nope, its fairly well established that goo is from MD clevage.  The colder the temp, the less cleavage, so indirectly, I suppose it's related.

#3  You are most ceratinly better off with DMF or chloroform than GAA.  Theres a post in Serious Chem.  "Bromosafrole Breakthrough" that in clear referenced terms says that GAA does dick to inhibit MD cleavage and that solutions in DMF were shown to be stable for several hours.  Osmium made the deduction that chloroform would be comparable to DMF, my experiments seem to indicate hes correct.  Hell, chloroform is easier to get that GAA anyway, so why bother with acetic acid?

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Forgive me for being rude, but would it be possible to just pump chlorine gas through safrole to produce chlorosafrole in any reasonable yeild? I know it works with isosafrole for the dichloro derivitive.  Could the chlorosafrole be reacted with methylamine directly? With or without heat?  I know yeilds would be worse, but I'm not finding NaBr.

No, bubbling chlorine gas through safrole would yield 1-(3,4-methylenedioxyphenyl)-2,3-dichloropropane ("dichlorosafrole"), which I don't know of any good use for.

I thought the route to the dichlorosafrole was done by pumping chlorine gas through isosafrole not safrole.  The dichlorosafrole can then be refluxed with KOH to produce MDP2P in 60% or so yields.  If I can produce the dichlorosafrole straigt from safrole, that would make my life much easier.

do you have refs for this? it would definately be most kewl if that would work.

Maybe Safrole w/ HCl bubbled through it w/ PTC to form chloro safrole, then a reflux w/ [K/Na]OH?

What about:

safrole + Br2 ---> dibromosafrole
dibromosafrole + KOH ---> MDP2P

Does this really work? Surely I'd have heard about it before if it did...

Sweet dreams,
IudexK

It has been descussed, search.  I know the procedure works, what is PTC?  I'm going to dream with the whole idea this week, I'm planning on using chlorine gas, but that sucks and HCL would be tight.  All the procedures for the dichlorosafrole use isosafrole.  The question is can I just use strait up safrole.

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another Idea I had was puting bromosafrole through the Al/Hg with nitromethane.  The reflux conditions and methylamine would be there, but would the reaction have an affect on the bromosafrole other than it's reaction with the methylamine.  It would be really cool if this would work because bromosafrole would then just be like a lower yeilding MDP2P.  That would be OK though because I'd save the yeild lost in the reactions that I would use to get MDP2P. The whole dichlorosafrole to MDP2P thing yeilds not much more than 50-60% from the safrole.

Never heard anything about that KOH reflux to MDP2P, it'd be nice though.

I've seen refs for the HCl + safrole + PTC --> chlorosafrole reaction.  You will most likely indeed get chlorosafrole form such a reaction.  I'm not sure exactly which PTC to use those, or if it'll be OTC.  The only problems I might forsee is that the chlorine may be too sticky, i.e. it'll bond to the safrole too tightly for a room temperature amination to work.  I think the only way to aminate chlorosafrole would be a bomb type thing.  ...??

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yep, chlorosafrole is not readily aminated enough for a room temp. amination to bee useful.

ok, so dihalogenating a propenylbenzene and then refluxing it with KOH will yield the phenylacetone, albeeit in not very good yields. However, I think this would only work with isosafrole, not safrole.

PTC = phase transfer catalyst

Sweet dreamz,
IudexK

Rhodium? Are you sure safrole + Cl2 ---> dichlorosafrole? This seems ridiculously easy... why do ppl bother with p-benzoquinone etc. if all it takes is a halogen and KOH!??

The halogens will be in the wrong locations. You have to use isosafrole.

Question about the agents original procedure...
Why can't bromosafrole be refluxed with methylamine.  Why bother with the whole week long deal.  Would the methylamine not condense and just be driven off as a gas?  If thats the problem would a bomb work?  And would Fe/HCl hurt the bromosafroleIf thats the problem would a bomb work?  Could nitro+bromosafrole+Fe/HCl simply be bombed to get the goodies?

Sure, MeAm reflux will work fine.  MeAm bomb will work fine too.  Probably even work better. 

I doubt that Fe HCl nitromethane and bromosassy in a bomb will do anything for you.

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from elusis' methylamine faq
Assemble a 500mL RB flask with claisen adapter, thermometer down the center to read the liquid temperature, and reflux condenser with a cork and tube leading to a beaker of 1M Hydrochloric acid. Drop a stirrer magnet in, then add 105g of 40 Mesh Iron filings, 225mL of water and 1g of Ferric Chloride. Next, add 35mL of concentrated Hydrochloric Acid ("muriatic acid" is ok). When the bubbling ceases, add 31g of Nitromethane.

Heat the reaction mixture to 100°C and hold for 14 hours. A temperature regulator is necessary if using a heating mantle, else use a large boiling water bath (if you will be doing it overnight, so it doesn't run out).

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All that is going on here to convert the Nitro to Methylamine is Fe, FeCl, HCl, and Nitro being heated to 100° so that part would work I don't see why bromosafrole would interfere with that reaction.  The resulting methylamine would react with the bromosafrole given reflux conditions.  So where's the problem?  Only one I can see would be the Fe or HCl interfering with the bromosafrole + methylamine reaction.  This reaction would be a little bit similar to the Nitromethane Al/Hg.  Think of how easy it would be.
Safrole + HBr --> bromosafrole
bromosafrole + Fe + HCl + nitromethane --> MDMA
I'll try it this week unless you can give me a good reason not to.  Please comment.

Ferric chloride is FeCl3, not FeCl or FeCl2..  you didn't mention using it in your post, so were you planning that Fe and HCl will form the FeCl3 in situ?  That is your flaw.

If you've got FeCl3 laying around then it might work excellently.

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SWIM has a feeling that if conducted at high temps as in bomb, this rxn will produce unwanted side-products which do not occur or occur to a much lesser extent if done at room temp. FeCl3.6H2O is available cheap form electronic supply places for etching.

So, am I to understand that if you add a halogen to a propenylbenzene, and reflux the formed dihalo- derivative with KOH, you will get the phenylacetone? If this is true, the implications for clandestine chemistry are staggering!  

Sweet dreams,
IudexK

Can the FeCl₆.H₂O be used directly or does it need to be heated to remove the .6H₂O?  What if instead of a bomb, I just refluxed?  Elusis' post says to bring it to 100° maybe I could take the mix there for a while, and if it's not a good reflux take it up after the methylamine has been formed.  Ohh how fun.  Yes, the dihalo thing is cool.  I wonder if I could just mix Br2, with the isosafrole to get the appropriate dibromo compound.  Hmmmmm...  

Iudexk: Yes, that is the implications of the japanese journal at the top. If someone could find the primary reference for this, we would all be grateful.

Why is there no japanese/chinese speaking bees on this board? You account for 20% of the world's population!

the choice of a solvant can give your reaction some drection, i think
could ethyl ether be use as chloroform?