posted 08-01-99 08:33 PM         

What about diluting with, say AcOH? If one dissolved the safrole in AcOH, then added concentrated H2SO4, problems with polymerization, etc. could be avoided, since the AcOH would act as a sort of heat sink. The acid addition to the olefin would still go as planned, though there may be an added benefit in that rather than the easily isomerized alcohol being produced, the acetyl ester, MDP-2-POAc, could be the favored product.

Quench w/ H2O, extract w/ DCM. Acids are then removed as before, and in the Base wash, deesterification could be undergone (though perhaps not necessary.) What do you think?

posted 08-02-99 07:37 PM         

Hydration works, and if esterified, its stabilized a bit more. I think this may be the key.

posted 08-03-99 01:40 AM         

You're new, and the mistake was made by Strike him/herself, but "borohydride" in the sense you're refering to, is NOT a catalyst. Its a reducing reagent. Sorry its a mistake that's senselessly propagated, and its a pet peeve of mine.

Secondly, ethics has EVERYTHING to do with it. In my state, we have more lakes and rivers than anybody, but a large number are filled with so much mercury that the fish are dangerous to eat. When mercury gets into the human body, it slowly kills a person inside-out, with all the classic heavy metal poisoning symptoms, plus the added bonus "mercury madness". That's what ethics has to do with it. In the Al(Hg) reduction method, which is bad, but at least only a tiny amount of mercury is used in comparison to the amount used in the oxymercuration-demercuration method. If you don't feel a little moral queasiness about this, you're either being ignorant, or there's something wrong with you.

Mercury is bioaccumulative, meaning that the higher on the food chain you are, the more mercury you will accumulate in your body in a contaminated environment. Never mind mercury-sensitive species of birds, insects, plants, and fish. Humans are pretty much the tippy-top of said food chain, meaning that mercury you're feeling unashamed about dumping is gonna find its way into the bloodstream of timberwolves, bald eagles, your friends, yourself, and your family. Ever seen heavy metal poisoning? Loss of hair, teeth, lesions, immune system problems, cognitive disruptions: not pretty. Improper mercury disposal is your contribution to this.

Mercury doesn't just go away; Hg2+ doesn't disappear once its released. It doesn't decompose. It stays that way. Tossing it down the drain may put it out of the direct line of site, but all it does it let it leach into some poor community's soil and water downstream, and eventually it finds its way into everything.

This isn't hyperbole. Its not pseudoscience. These are the facts, and yes you should take them to heart. You DO NOT need to contribute to this problem. Period. You do have access to more environmental alternatives, including the ever-frightening choice of (*gasp*) simply NOT making MDMA.

Let's face it, you sound like you're a ways from acatually seeing any homemade honey. Why not take the time to find a method that isn't gonna aquire you as much nasty Karma? I garuntee, if you put your mind to it, you'll find easier methods with better yields.

posted 08-03-99 04:23 PM         

Oh-oh!

posted 08-03-99 05:31 PM         

1. Is a clandestine chemist going to take his Hg sludge to a "destruction or recycle plant"?

Nope.

2. So what are they going to do with it?

Put it down the sink.

You people have to realize that 99.9% of these people want the drugs and not the manufacuting/research/lab experience. Promoting the use of Mercury compounds will only put more Mercury in the environment.

I don't care if its an acceptible industrial process. I don't care if it gives theoretical yields of 99.9%. The fact of the matter is that if someone of reputation (PK) endorses the use of Mercury compounds, then others will use it.

I mean these people that you are telling this works to, are the same people who want you to tell them where HCl is. And you expect them to find a 'destruction or recycle plant' ...
Give me a fucking break.

Stop it Seigfried, and listen to the drone. He is right and you need more experience.

posted 08-04-99 06:35 PM         

Now having said that, I think its also wrong to give bees out there (especially the newbees and the wannabees) the wrong impression about Hg compound usage for Honey production. First off, I think a very common misconception forms among the newbees and that is the idea that using mercury makes for almost perfect, easy and high-yielding synthesis and that the only trade-off is the Hg waste produces. They figure, look I need the cash, then once I'm set, I'll learn "cleaner" forms of underground chemistry. This is (and I'm speaking from experience here, and I think Siegfried will join me on this one...) categorically FALSE! Amino-mercuration and other such methods are NOT simple, NOT facile, NOT high-yielding (not as yet any way!) What they are is DANGEROUS, because the presence of H20 soluble mercury salts and even worse organomercurial intermediates involved. EXTRA EXTRA care has to be taken just not to accidently kill yourself, let alone poison the environment.

But having said that, a proven method (once developed and all bugs worked out) involving mercury could verywell be useful, without being environmentally unfriendly. Proper recycling and/or passivisation could be incorporated into the work up. But once again, it is not for the beginner chem-hack, not because it's that much harder than any other synth, but because there is that much slimmer margin for error which can result in permanent harm to you, your friends, or the environment.

So the moral of it all, newbees and whanabees, cut your teeth on some easier and more friendly synthesis that are out there (Especially Brightstar's great outline). Old bees and reverend bees, lets not turn away from a path just because of the Hg word now!

PS: Siegfried, it is in the area of Direct intermolecular amino-mercuration that I have experience. I'll be happy to share my data with you.

posted 08-05-99 10:34 PM         

Aw shucks. ReFlux aside, I'm gonna asume you meant me, and be flattered.

Siegfried,

Es scheint mir von deinen Posts, dass Du Deutsch als deine Muttersprache hast (obwohl, es war ein bisschen offensichtlich mit einer Namen wie "Siegfried".) Wie ist es, dass in einem Land so umweltbesorgt wie Deutschland, jemand Drogenchemie schaffen kann? In Deutschland, kann man echt Chemische Muehl zum Organisation, wie du beschreiben hast, schicken? Hier, haben wir nicht so einen Luxus -- hier, muessen wir andere moralischen Methoden finden, was mit unseren Chemikalien zu tun.

Oxymercuration may be modern, but it isn't exactly widespread, precisely because of waste issues. Its only used where nothing else will do.

I've found some interesting additions of sulfonates and other acids across olefins, as written in another thread. I'll post those when I've gone through them all.

posted 08-11-99 12:44 PM         

I would like to pinpoint out something which is worrying me for sometime now.
It looks more and more as if many people posting here, consider it as a pure american board. They fail slowly to consider the rest of us as non-americans, who live in different circumstances and/or repression measures.
Some entering as newbee's are forced to accept motivations for synths, which in their specific circumstances are ridiculous, for clear and obvious reasons.
They have access to a much wider arsenal of chems and materials then the USA bee's, so, they are without knowing, for the fact they are new here, lead on a, for them, wrong path.
The need for you, americans, to find complicated methods to avoid the unpleasent acquaintance of the surpressive methods of one of your three letter organisations is also obvious.
But, would you consider to evaluate a bit more the possibilities for the rest of the world population ( that's the other 95 %) to obtain the desired endproducts?
I mean also devide your attention to the other well known methods, but not discussed here to the full extend.
I try to think global, many of you are stucked in chauvenistic thinking( I know, pressed by circumstances beyond your wishes).
But if someone proposes a good working synth, but with precursors out of reach for our american friends,it should get more attention then I see now.
Btw, its also obvious that you do not fall in this category, but many others do, so I hope they read this once, and give it a thought.
Sometimes different pathes can deliver surprising new techniques, applicable again also for american aquisition purposes.
Think global, once again, do not make the same mistakes as your politicians made repeatedly for 50 years now. They refuse to try to impersonate themselves into the minds of other world citizens, and slowly lost contact with the outside world, and still do not understand what exactly they did/do wrong.
They say they want to help, but in reality want to exploit..... LT/

------------------
EMOTIONSwill always beFREE!

posted 08-25-99 02:12 AM         

have you came up with anything yet?

posted 08-25-99 01:00 PM         

I'm asking that you use way less than a gram of it. I calculated once th e amound needed (by surface area calculations) and the amount needed for 40g of Al was ~0.003g or Hg(OAc)2. I also asked you not to put it in the environment. I am in the unique position that I work around chemicals, and I can dispose of it properly.

Oxy-mercuization requires a slight molar excess of Hg(OAc)2 ... so if you wanted to process one mole of saf (160g) then you'd have to put in 320g of Hg(OAc)2.

Can you see the difference now?

Fine ... I concede that you can get *most* of it back (95% or so) by nitration with nitric acid ... nitric acid is pretty expensive. and if you wanted to to it again, youd have to put the Acetates back on. In each of these steps you will loose +5% of the Hg. You are going to wash, and put it down the sink, instead of keeping all the washes and disposing properly.

So at the end of a one molar batch you are going to loose: Lets make this conservative and say there are three steps from Hg(OAc)2 --> Hg(metal) --> Hg(NO2)2 --> Hg(OAc)2.

This is a horrible approximation because ther are filtration, distillation, and other purification steps in between EACH of them in which you loose Hg.

100%-5% = 95%
95%-(5%of95%) = 90.25%
90.25%-(5%of90.25%) = 85.74%

So you get 85.7% of your Hg back. Out of 320g starting ... thats 274.3g.

Where did the 45.6g go?

Which is worse? 45.6g or 0.003g?

I know you bees. I am one. When you get the product are you going to?

a. Clean your space, mark your bottle of product, and put it on the shelf?
b. Start reading more of Shulgin's works?
c. Become completely facinated with bio-chemistry, and apply to a Ph.D program somewhere?
d. Party like hell for two weeks, and neglect your messy lab top?

My money is on d. Everytime. I did it (but I cleaned it up afterwards) and, all of you new bees will do it, too.

Quit kidding yourself.

Anyway, I did a few experiments a while back on the 2-ol. It definately formed. Keeping it cold seems to be a good thing. Anyone know of a low temperature oxidation? -ol to ketone?