Author Topic: Questions Pertaining to Bromosafrole to MDMA - THANKS :D  (Read 221 times)

ImAMANGUYS

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Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« on: June 21, 2012, 03:25:53 AM »
Okay, so this is me attempting to do my research :D
Originally i was interested in the Dr. Drool synthesis as a nice little way to create MDMA. The Pdcl2 price/attainment is an obvious blockage in the perfect plan Dr. Drool seems to set out.
So upon further investigation I found a writeup in the Rhodium Archives which mentions Sassafras Oil --> Bromosafrole --> MDA/MDMA

LINK MOTHER TRUCKERS:
http://www.erowid.org/archive/rhodium/chemistry/halosafrole.txt

Im looking specifically at the syntheses proposed by Ritter and Jon.
A couple of questions arise from my reading of the context. They may be obvious to you, but I'm still learning and have obviously UTFSE, so any help would be appreciated.

QUESTION 1:

Referencing this passage from Ritter:

The final mixture gets 500-1000ml of water added. The crude bromosafrole
which settles to the bottom is seperated without adding any organic
solvent. If you cool it it gets pretty sticky and syrupy so the water layer
can be just poured off.

and this from Jon:

Once all the acid in the product is removed, the ether must be
removed from it. This is important because if the ether were allowed
to remain in it, too much pressure would be generated in the next
stage inside of the bomb. Also, it would interfere with the formation
of a solution between the product and methylamine or ammonia. It is
not necessary to distill the product because with a yield of over 90%,
the crude product is pure enough to feed into the next stage. To
remove the ether from the product, the crude product is poured into a
flask, and a vacuum is applied to it. This causes the ether to boil off.
Some gentle heating with hot water is quite helpful to this process.
The yield of crude product is in the neighborhood of 200 grams.

     With the bromo compound in hand, it is time to move onto the
next step which gives MDA or MDMA. See Chemical Abstracts
1961, column 14350. Also see Journal of the American Chemical
Society, Volume 68, page 1805 and Journal of the Chemistry Society,
part 2 1938, page 2005. The bromo compound reacts with ammonia
or methylamine to give MDA or MDMA.

My question being, are both of these "Bromo Compounds" the same compound? if not, how do they differ? Can Ritter's so called "Crude Bromosafrole" be used in the pipe method later described by Jon when adding Methylamine?

Also, pertaining to Jon's sythesis, how is the vacuum applied to the flask? Im running into confusion with visualization...  :-\

QUESTION 2:

I have read in another source, which momentarily slips my brain... :( That 91% Isopropyl Alcohol, or 99% Isopropyl Alcohol if need be, can be used in place of Ethyl Ether (ether, diethyl ether) with equal or sometimes greater results...

Now I hope I have not made a fool of my self for a such a question as I am a beginner.
If it is "replaceable," could it be replaced here:

In Jon's Synth:

The reaction mixture is now poured onto about 500 grams of
crushed ice in a 1000 or 2000 ml beaker. Once the ice has melted, the
red layer of product is separated, and the water is extracted with about
l00 ml of petroleum ether or regular ethyl ether. The ether extract is
added to the product, and the combined product is washed first with
water, and then with a solution of sodium carbonate in water. The
purpose of these washings is to remove HBr from the product. One
can be sure that all the acid is removed from the product when some
fresh carbonate solution does not fizz in contact with the product...

Would the Sodium Carbonate solution be best if fully saturated?

Okay,

LAST QUESTION:

and this should be fairly obvious for those more skilled than I am.

Is Jon suggesting that the same process he's using from Bromosafrole --> End Product will produce MDA with the use of Ammonia and MDMA with the use of Methylamine?

OKAY! PHEW! enough questions for now... More research is following. Thanks for those who have the patience to read and reply :)

« Last Edit: June 21, 2012, 03:29:29 AM by ImAMANGUYS »

myCH3

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #1 on: June 21, 2012, 03:49:46 AM »
Welcome always good to see a new face, unfortunately I can only answer your last question "Is Jon suggesting that the same process he's using from Bromosafrole --> End Product will produce MDA with the use of Ammonia and MDMA with the use of Methylamine?"  and the answer is yes

fresh1

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #2 on: June 21, 2012, 05:23:47 AM »
Quote
ow is the vacuum applied to the flask?

yoou need to have suitable 'equipment' (preferably some nice quality borosilicate vacuum flasks) it's hard (nigh impossible) to whip up a ghetto vaccum distillation setup, whereas a filtering setup is pretty easy.  ANY leaks causing you to lose vacuum will have you pulling your hair out and in tears when this happens at a crucial part of your dreams ;)

At the bottom left of this page is a buchner funnel sitting in a 'vacuum filter flask' (erlenmeyer flask=flat bottom conical)

 Have a look at the clear plastic hose going into the flask-this is the hose to the vacuum pump....have a good read Man ;)

http://en.wikipedia.org/wiki/Laboratory_glassware 

Quote
are both of these "Bromo Compounds" the same compound
in a word, "yes"  :)

 And Mymethane has answered the last question accurately ;)

 It's great to see new wasps jumping in and getting the feet wet I would suggest however you get yourself a copy of

"The Lab Survival Guide" by ? Zubrick (?) or something similar asap to help yoou 'picture' things a bit better :D

 I hear it's a very good easy to understand and quite a good read ;)...or you can UTSE and cobble together bits and pieces from all over

  Good luck with your dreams mate :) 

ps. why dont you do a little intro for us so we can say G'day ;D
"Curiosity is a gift"

Wizard X

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #3 on: June 21, 2012, 05:29:14 AM »
I've answered your questions at The Collective.
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

atara

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #4 on: June 21, 2012, 07:53:43 AM »
http://its.goofyti.me/u/http://www.google.com/patents?id=pCJyAAAAEBAJ&printsec=abstract&zoom=4#v=onepage&q&f=false

This patent claims that, among other things (palladium), silver is an effective catalyst for hydrohalogenation. That could be very convenient -- the major present issue with the hydrohalogenation of safrole is that it is very slow. Nickel is effective as well, but nickel will reduce hydrogen, which is bad. I've heard such things as FeCl3 and BaCl2 suggested as well.

Finding an effective catalyst for this otherwise touchy reaction could make it much more accessible... if nickel works, maybe copper(I) will?
« Last Edit: June 21, 2012, 08:00:52 AM by atara »

ImAMANGUYS

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #5 on: June 21, 2012, 10:25:27 AM »
ps. why dont you do a little intro for us so we can say G'day ;D

Okay  ;) Hello all. I'm just a fellow dreamer, somewhere in between. I'm addicted to learning... What can i say? That's what i hope to do here.

yoou need to have suitable 'equipment' (preferably some nice quality borosilicate vacuum flasks) it's hard (nigh impossible) to whip up a ghetto vaccum distillation setup, whereas a filtering setup is pretty easy.  ANY leaks causing you to lose vacuum will have you pulling your hair out and in tears when this happens at a crucial part of your dreams ;)

At the bottom left of this page is a buchner funnel sitting in a 'vacuum filter flask' (erlenmeyer flask=flat bottom conical)

 Have a look at the clear plastic hose going into the flask-this is the hose to the vacuum pump....have a good read Man ;)

http://en.wikipedia.org/wiki/Laboratory_glassware 

Thank you! Im aware of how to form a vacuum with both setups (buchner and distillation), but was trying to imagine... Would a simple stopper in a conical flask with a vacuum attached to the nozzle "bubble out" the ether? or would vacuum distillation be a more suitable option... Sorry if that sounds dumb  :-\ you live and you learn  :)

YES :D I've downloaded the Survival Guide and read thoroughly through the distillation section already... Guess I'll read it fully indepth...

I've answered your questions at The Collective.

Thank you again Wizard X, you were very helpful and I've replied promptly to your post... With a few more question I might add  ;) :P Sorry, can never learn to much. Science is well.... a science... hhaha

http://its.goofyti.me/u/http://www.google.com/patents?id=pCJyAAAAEBAJ&printsec=abstract&zoom=4#v=onepage&q&f=false

This patent claims that, among other things (palladium), silver is an effective catalyst for hydrohalogenation. That could be very convenient -- the major present issue with the hydrohalogenation of safrole is that it is very slow. Nickel is effective as well, but nickel will reduce hydrogen, which is bad. I've heard such things as FeCl3 and BaCl2 suggested as well.

Finding an effective catalyst for this otherwise touchy reaction could make it much more accessible... if nickel works, maybe copper(I) will?

Thanks for the suggestion atara, but I've researched Bromosafrole ruites in order to avoid buying metal salts. Expensive  >:(

lugh

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #6 on: June 21, 2012, 03:18:26 PM »
Chemistry is our Covalent Bond

ImAMANGUYS

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #7 on: June 21, 2012, 04:02:43 PM »
Please read:

http://127.0.0.1/talk/index.php/topic,828.0/all.html

http://127.0.0.1/talk/index.php/topic,1697.0.html

http://127.0.0.1/talk/index.php/topic,1833.0/all.html

and numerous other threads that can be found elsewhere on the internet  8)

Thanks lugh! I didnt see one of these! :)

Could anyone answer my question about replacement of ether with isopropyl i asked in the original post?

Polonium

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Re: Questions Pertaining to Bromosafrole to MDMA - THANKS :D
« Reply #8 on: June 21, 2012, 05:31:34 PM »
I'm not sure about IPA but I know dichloromethane works well for extracting bromosafrole after the bromination in GAA. I think Jon also said that TCE works if that's available to you. One advantage of using DCM is that it is easy to remove from the bromo product at low temperatures.

I'm not sure how you are planning on performing the amination, I would suggest you have a look at Sn2 reaction instead of the Sn1 reaction in near anhydrous IPA that Jon uses. One of the advantages of the Sn2 is that the methylamine free base can be formed in situ by the action of triethylamine or some other non nucleophilic base on methylamine in DCM. This avoids the use of methlamine gas. I have posted the referances for this reaction previously and it is on the rhodium archive, but the amination is not being applied to this substrate.

Happy dreaming, experimentation is king.

Edit: Here is my original post about the amination in DCM. http://127.0.0.1/talk/index.php/topic,1833.msg31231.html#msg31231. It includes a reference for the synthesis of mephedrone from its bromo analog. Yield is only 50% but this should increase with iodosafrole as it had a better leaving group.
« Last Edit: June 21, 2012, 08:40:49 PM by Polonium »