safrole+bomb?happy chinaman

[Chinaman]

Im having a little debate in my head
could one go about throwing safrole and CH3NH2 into a bomb
to yield mdma without first converting safrole into bromosafrole or mdphenacetone?
greatly appriciate any input into my delema



Remember its illegal we have to get rid of it... puff puff puff

[psychokitty]

No. 

Not yet, at least.

--PK

[PolytheneSam]

Some one I know tried it with 40% methylamine solution, sassafras oil (without purification), a drop of sulfuric acid as catalyst and some transition metal salts as catalyst based on US patent 4937383.  This patent only gives examples of reactions using isobutene, but it looks like it follows Markonikoff's law where if you add R-H across a double bond, the R group goes to the carbon with the least hydrogen atoms.  He tried smoking the residue after the reaction and then later he tried it orally after letting it air out for a while and he found it to be psychoactive.  He saw the brightest colors he ever saw, experienced euphoria and an MDA like high which he was familiar with before.  So if that test was good enough I would say that yes it will work.  I don't know what the yields are.  The sassafras oil was at least 25 years old but still had a very strong safrole smell to it.
You can look up US patent 4937383 using this web page:

http://www.geocities.com/dritte123/PSPF.html

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[Chinaman]

Thanks man yea i was thinking about Markonikoff's law that the radical would attach to the most stable carbon
and the secondary C group looks to be the most stable
Thanks again ill have to follow up on the link and do some more research

My cat keeps talking to me. Should i answer or or finish eating this piece of paper?

[foxy2]

Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN

Thanks for all the kick ass patent work Sam!!!


Do Your Part To Win The War

[PolytheneSam]

I think Chem_Guy was the first one to post things about direct amination.  He listed one or two patents in his thread.  Here's a list of patents on direct amination of alkenes.

2397705 2501509 2501556 2518528 2627526 2984687 4454321 4827031 4929758 4937383 5107027 5900508

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[jim]

Funny, I tryed posting in this thread yesterday, but I guess it never went thru....  ?

I thought that the high temperatures of this patent would cause isomerization of the allylbenzene double bond forming a propylbenzene. 

The patent does seem to put the amination with a Markinokov addition (nulcleophile to the most substituted carbon).  Which means that the amination works for only allylbenzenes like safrole (if at all).

If you want I can dregde up my old articles and threads, but I think it is all on my website (

http://chemguy.homestead.com

)

[PolytheneSam]

Yeah, I never thought about isomerization.  I thought it needed stronger bases like KOH and CaO.  Ammonia and methylamine aren't as strong. The bomb process also seems to produce tar, too, (I don't know if the amine is a solid or not) so it looks like you have some competing reactions.  Maybe this type of process is good if you already have a bomb or autoclave and just want to do some quick experiments with various essential oils.

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[jim]

I have begun to look at the patents again.  Patents 4,937,383 and 4,827,031 look good.

HOWEVER, I still am wary about the isomerization, but they look easy to test.  # 4,827,031 doesn't look as promising, the pressures are higher, it quotes use for compounds 2-8 carbons long, and uses slightly higher temperatures.

# 4,937,383 looks more promising.  The pressures seem attainable.  The yields are well below 50% though.

US Patents # 5,107,027 and # 5,900,508 seem not too good.  The zeolites, if you can get them, are pretty acidic and might cause ether cleavage and will cause some polyermization.  The patents do state however that they can aminate compounds 2-10 carbons long, even with aryl groups.  The patent DO NOT tell you weather the addition id Markinokovian though, which is of great importance.  If anyone can figure that out please post it...

[thunker]

How about this untested variation on your idea.  I don't know if this is original or not -- I've never found it in the literature.  If it doesn't work, I'd appreciate knowing the reason why.  If it does work ...  

[foxy2]

That is an awsome idea, add a touch of acetone~1ml to aid in the decarboxylation maybe.  And some ammonium sulphate catalyst.

Those pipe bombs scare the shit outta Foxy too though  

Someone needs to try this.
You could potentially take undistilled sassy and make E with NO glassware and very little apparatus


Do Your Part To Win The War

[Day_Trippah]

LOL i like the part about the terrified chemist. I have to say though that this is the coolest shit i have ever read. if this works and it looks like it can, the DEA just got buttfucked.    so how 'bout it chemists? by the way i read somewhere that sassy is illegal now? is that true?

             

[PolytheneSam]

The temperature is what drives the reaction not the pressure.  The reason for the bomb is to contain the water and ammonia (or amine) because it would evaporate without it.  OK, if you start with 20 g of CO₂ as dry ice in your modification, thunker, what would the pressure be in a 250ml bomb when it turns to a gas at 32-49°?  Use the ideal gas equation, PV=nRT.  Also, if you want you can try Van der Waal's equation, too.

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[foxy2]

Yea Sam has a point.  It would bee best to use a high boiling inert solvent for the bomb instead of CO2

Hmmm
para-Dichlorobenzene?
Insoluable in water, otc, easy to wash away with dcm in A/B extraction, boils at 173.4C, melts at 56C.  Heat to 190C or so and away we go.  Pressure probably wouldn't bee an issue becasue the para should stay liquid up to 200C under minimal pressure.  This idea is COOL!!!


Do Your Part To Win The War

[jim]

Halide replacement by the amine would be a problem with para-dichlorobenzene...

The pressure in the "bomb" with raise the boiling point of the solvent.  The CO2 could in a a liquid form (supercritical actually) at these high temperaures if the pressure was great enough. 

I have grave reservations about using clandestine chemistry bombs, I would fear for my life.  I would also put at least 2  pressure saftey blow-off valve and a pressure release valve to release pressure when taking off the lid.

[PolytheneSam]

The vapor pressure of water at 250° C is 27 atm.  In P. Chem. lab we were filling bomb calorimeters with 25 atm of O₂ before igniting the samples.

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[Day_Trippah]

So are you saying the bomb would blow?

             

[foxy2]

sam those bombs in pchem lab are fucking thick and heavy duty!!!!

Do Your Part To Win The War

[PolytheneSam]

So are you saying the bomb would blow?

No.

http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0

http://www.privacy.org

[Day_Trippah]

oh