posted 07-01-99 10:08 AM         

I have seen it, and it is true.

A friend recently utilized some ancient polish refs that said 48% HBr WILL add to olefins like safrole with NO PTC's and NO other additives.

He used homemade 48% HBr and singledistilled olefin. Stirred for 7 days and achieved over 90% yield.

Pulled out the bomb, added 20 g of his bromosaffy and 25 g MeAM.HCl, neutralized the salt w/ NaOH, and cooked it @70 deg. for 16 Hours.

Yield over 19 grams.

Most of this stuff is overkill. (underground)

posted 07-01-99 10:34 AM         

The amine is present in a nearly 10x molar excess, ensuring high yield.

This is one of the most researched reactions in the world.

It has been clouded and mystified by the
'Powers that be'

posted 07-01-99 01:16 PM         

So what do you attribute the failings of the past? The Time factor? hummmmm .... Heavy stirring? The bromo-addition was done at RT?

What made you choose the 48%? All that was availiable? Made your own?

What was the concentration of your MeAm? Water solution? Alcohol? What pressure was the bomb? SRV?

Droney will ask for a ref ....

Well it is a 'standard' reaction and I have wondered why it didn't work ...

posted 07-02-99 07:29 PM         

Questions:
1. What temp did you combine the HBr and Safrole?

2. Safrole is not mincible with aqueous HBr. How fast was this stirring? What was the ratio of acid to safrole?

3. Did the layers become more or less mincible near the end of the rxn.

4. What was the color progression during the hydrobromination?

5. Was the Bromosaf treated with base then distilled as in the ref? If so, what vac/temp did it come over? What color was it?

posted 07-04-99 03:33 PM         

Let me add credablity to your claim sir.

I posted this a while back in the Novel Discourse forum. Its title is "...(MMDA) Derivitives Synthesized from Nutmeg Oil..."

Here it is,...

The full name of this article I am going to paraphrase is "Analysis of
1-(3-methoxy-4,5-methylenedioxyphenyl)-2-propanamine (MMDA) Derivatives
Synthesized from Nutmeg Oil and 3-methoxy-4,5-Methylenedioxybenzaldhyde" . It is in
the journal of chromatgraphic science, Vol. 34, januuary 1996.

The Nutmeg oil is a methanol extract.
(Quotation)
"BROMINATION REACTIONS
A suspension of nutmeg oil in 48% HBr was stirred vigorously at room tempature for 7
days. The reaction was then quenched with the addition of crushed ice and extracted
with ether. The ether extracts were combined, washed with water, and evaporated to
dryness under reduced presure , and the resultant product oil was analyzed directly by
GC-MS.
AMINATION REACTIONS
The crude bromination product was disolved in methanol containing methylamine and
stirred for several days. The reaction mixture was evaporated to dryness, and the
resultant oil was disolved in 10% HCl. The aqueous acid solution was washed with ether
and then made basic (pH 12) by the addition of NaOH pellets. The aqueous base
solution was extracted with ether, then the combined ether extracts were evaporated
to dryness under reduced pressure. The resulting oil was analyzed directly. "

In another arctile concerning this same topic except the oil was safrole. (Journal of
Chromatographic Science, Vol. 29, april 1991 page 169) It says

"... analysis showed the bromination occured slowly and required approximately 7 days
to consume most of the Safrole.... The results of the present study clearly shows that
MDMA and related designer drugs analogues of MDA can be prepared by amine
displacement of bromosafrole obtained via bromination of the organic steam distillate of
the roots of the saasafrs plant."

That same article gives the same reaction method except with safrole with the numbers
being... 5 grams of sassafrs oil in 25 mL of HBr (48%). Extracted with two 50mL
washings of ether. The crude bromo-product was 2 grams in 100 mL of methanol
containing 40% methylamine (25mL). It was stirred for 4 days, reacted with 50 mL of
10% HCl and washed with two 50 mL of ether. Etc....

NOTE: This reaction can also use ammonia instead.
CHEM GUY
Member
posted 06-24-99 04:06 PM

Does anyone have any info on the bromination with a PTC (Phase trransfer catalyst)?

posted 07-06-99 10:43 AM         

Not-me has never tried it ... but you are right ... it must work. I think most bees are impatient ... And that has been their down fall ...

posted 07-06-99 11:55 AM         

If you just by yourself a magnetic stirrer and wait the required time (~1.5 weeks) you WILL get XTC. The yeilds are a little low (~50%-25%). But when weighted against the cost of making it yourself or buying, god knows what, from Mr Narc, it sounds pretty good.

Now there is no 100% yeild method so stopp looking for it.

posted 07-08-99 12:57 PM         

BUT, ....

re; failings of the past; using NH3 instead of MeAM, its just too volatile.

temp@ HBr add'n- 25 c.

set to 6 on my Thermolyne stirplate.

red-burgundy.

Finally, the bomb idea is NOT sketcchy.

Its EZ as hell.

Pressure threads, y'know.

And its as close to 100% as you'll ever see.

Bright Star- I'll e-mail you soon.

ChemHack- You too.

Most of you others, too...

posted 07-08-99 08:07 PM         

Ohhh, I got to be reading this incorectly, There has to bee a catch, It could NOT be this easy.

I am off to the library to see if it has the referenced material.

Any one ever grow their own sassy plants? This sure sounds promising for the backyard type of guy (like me)

How did your "friend" manufacture the HBr?

posted 07-10-99 02:32 PM         

By the way, why do you want to know? How hard would it be to make the NH4O(CO)CH3 into NH3 or NH4OH any way?

Why not get the methanol and add that fertilzer crap, NH4SO4, to it. Add NaOH to liberate the NH4OH and the Na2SO4 will precipatate out.

posted 07-10-99 02:35 PM         

NH4SO4 should read (NH4)2SO4
the formula shoyld read:

(NH4)2SO4 + 2 NaOH + (in alcohol) --> Na2SO4 + 2 NH4OH

posted 07-10-99 08:15 PM         

"The crude bromo-product was 2 grams in 100 mL of methanol
containing 40% methylamine (25mL)."

This was concerning safrole not nutmeg extract, but I'm sure it will work for nutmeg as well.

And yes IsoPropylAlcohol would work just fine, if it dissolves both products. ( the bromo- and NH3 or NH2CH3 or the like)

posted 07-16-99 02:43 PM         

ROR + HI, cold --> ROH + RI

I don't know how it splits asymetrical ethers.

posted 07-16-99 06:14 PM         

Also, it is possible to iodate alkenes w/ just iodine and Alumina.

posted 07-16-99 06:19 PM         

What I'm getting at is that at higher temps the addition of HBr proceeds via free-radical process and not in the desired position. How can you be sure that you did not simply amminate this wrong bromo compound (who's resulting amine is mildly psycho active)?

posted 07-17-99 03:52 PM         

By the way my article says at room temp, (+25 C).

Concerning the need for water for the clevage of ethers,...

posted 07-17-99 10:03 PM         

Gee Dr strange glove,
If you could just lay it on the line.!

with write-up,
THAT SURE WOULD BE SOMETHING.
It would be the ultimate recipe.

6 reasons why you should bromonate safrole,.

1) your safrole can be dirty(Within reason)
2) No isosafrole
3) no Pdcl2 ordering
4) No HgCl2- that sure would be nice
5) no p-benzoquinone-
6) even no Dimethyl formamide( DMF)

Seeya Dudes,

Who's gonna be the bromo man?

posted 07-18-99 01:40 AM         

Now it's as simple as borrowing a bottle of nutmeg, brominating by stirring with aquaous HBr, then throw it in Mom's pressure cooker for a few days, and presto, instant "XTC".

if it's written down then it's gotta be true.

e(gladI'mnottheonlyskeptic)quarius

posted 07-19-99 08:37 AM         

Several people have been praising this brimination/debromination pathway to ecstacy because it can be used with nutmeg extract as well as safrole. But if myristicin is the precursor in nutmeg, wouldn't the final product have a methoxy group hanging off of it, making it different from MDMA? Is the term "ecstacy" used here to denote MDMA as well as its derivitives?

posted 07-20-99 12:42 AM         

The DMSO reaction involving bromide's with h2so4 WILL LEAD TO PROBLEMS,
I have data that suggests that the Hbr is oxidised again by the h2so4, giving elemental bromine,
This though can be rectified by using phosphoric acid instead,.
I believe this might be one of the contributing factors that is giving everybody such inconsistant results.

HBR- the problem child,
How about passing a stream of H2S into some bromine and water, no good I'm sorry,
You'd then have to seperate the bromine from the Hbr,.I hear you say.
Fuck that,.

DR weirdmitts, please respond.

Don't just.......

posted 07-20-99 01:21 AM         

Strikes post, re: superior Hbr..., gives no success at all, infact it ends worse than it started.
Are you comments fueled by optimism, or fact.
Just because some girl named pugsley write's some shit, it doesn't make it fact.

There is a rollcall over in the methods section on successfull bromination,
Nothing complete yet.

posted 07-20-99 03:00 AM         

2NaBr + 2HCl + H2O2 ------> 2NaCl + 2H2O + Br2

posted 07-21-99 02:13 PM         

I wanted you to read the post because it points out a textbook source and it also tells you some faliures.

First off I learned it that thread that refluxing is stupid, it fucks up everything.

Next, I learned that a PTC will definitly help out the process. You can even chloronate with a PTC. If you wanted you could chloronate with the PTC and then replace the Cl with I so it would be easier to replace with the amine group.

Thirdly, learn from others mistakes. You are right that just because someone writes something down it's so. But academic sources are different. I have academic sources.

posted 07-26-99 08:29 PM         

move on.

It's just not worth it,
Believe me, you reasarch it for about 20hrs, then you'll see why.