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    Subject safrole+bomb?happy chinaman   Reply  
    Posted by Chinaman (Stranger)  
    Posted on 04-06-01 08:12  
    Post No 182458  
   
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 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by psychokitty (Hive Bee)  
    Posted on 04-06-01 08:23  
    Post No 182461  
   
No. 

Not yet, at least.

--PK 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Master Searcher)  
    Posted on 04-06-01 11:05  
    Post No 182501  
   
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/ 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by Chinaman (Stranger)  
    Posted on 04-06-01 20:54  
    Post No 182574  
   
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?
  
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by foxy2 (Hive Addict)  
    Posted on 04-07-01 04:58  
    Post No 182603  
   
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 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Master Searcher)  
    Posted on 04-08-01 03:17  
    Post No 182689  
   
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/ 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by jim (Hive Bee)  
    Posted on 04-08-01 07:48  
    Post No 182755  
   
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/ ) 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Master Searcher)  
    Posted on 04-08-01 09:09  
    Post No 182775  
   
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/ 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by jim (Hive Bee)  
    Posted on 04-13-01 06:19  
    Post No 183698  
   
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... 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by thunker (Stranger)  
    Posted on 04-24-01 10:09  
    Post No 186323  
   
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 ... laugh

A HEAVY stainless steel pipe bomb is prepared.  The bomb is charged with safrole, an equimolar amount of glycine, some amount of carbon dioxide in the form of dry ice pellets, and a catalyst, as described elsewhere in this thread.  The pipe is flushed with carbon dioxide, then sealed.  The sealed bomb is heated to ~32-49 degrees C and held for several hours.

Here's the theory:

The carbon dioxide turns to gas, then the combination of the containment pressure and temperature causes the CO2 to enter the supercritical region, forming an excellent solvent for the reaction to follow.  Under these conditions, the glycine decarboxylates over the course of about two hours, yielding methylamine and more carbon dioxide, which adds to the solvent.  Finally, the methylamine and safrole condense, yielding, hopefully, MDMA.

When the reaction is complete, the pipe is cooled, first in air, then in ice water, then in acetone/dry ice.  The terrified chemist then carefully releases the pressure by unscrewing the cap.  The drop in pressure solidifies most of the CO2.  Once the pressure is released, the cap is removed, and the pipe is placed in a contained vessel.  A tube runs from the containment vessel through a beaker of dilute HCl.  First, the carbon dioxide vaporizes away, then any remaining methyamine vaporizes, and is captured in the HCl beaker and precipitated as the hydrochloride.  What remains in the pipe is hopefully MDMA freebase, ready to be purified and gassed.

crazy 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by foxy2 (Hive Addict)  
    Posted on 04-24-01 13:42  
    Post No 186387  
   
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 shocked

Someone needs to try this.
You could potentially take undistilled sassy and make E with NO glassware and very little apparatus
smile
Do Your Part To Win The War 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by Day_Trippah (Stranger)  
    Posted on 04-26-01 14:45  
    Post No 186940  
   
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. laugh so how 'bout it chemists? by the way i read somewhere that sassy is illegal now? is that true?
coolcoolcoolcoolcoolcoolcoolcool 		 
   
 
   
    Subject Re: safrole+bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Hive Addict)  
    Posted on 04-27-01 23:31  
    Post No 187303  
   
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/ 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by foxy2 (Hive Addict)  
    Posted on 04-28-01 01:37  
    Post No 187323  
   
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 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by jim (Hive Bee)  
    Posted on 04-28-01 03:04  
    Post No 187342  
   
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.  		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Hive Addict)  
    Posted on 04-28-01 03:26  
    Post No 187345  
   
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/ 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by Day_Trippah (Stranger)  
    Posted on 04-28-01 16:19  
    Post No 187508  
   
So are you saying the bomb would blow?
coolcoolcoolcoolcoolcoolcoolcool 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by foxy2 (Hive Addict)  
    Posted on 04-28-01 18:26  
    Post No 187548  
   
sam those bombs in pchem lab are fucking thick and heavy duty!!!!
Do Your Part To Win The War 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by PolytheneSam (Master Searcher)  
    Posted on 04-29-01 08:11  
    Post No 187679  
   
Referring to:

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/ 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman   Reply  
    Posted by Day_Trippah (Stranger)  
    Posted on 04-29-01 13:06  
    Post No 187753  
   
oh
coolcoolcoolcoolcoolcoolcoolcool 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman New   Reply  
    Posted by Day_Trippah (Stranger)  
    Posted on 04-30-01 09:54  
    Post No 187967  
   
SWIM will try it if someone would tell SWIM what the fuck glycine is and where/if SWIM can buy it and also the current statis on sassafrass oil legal/illegal
coolcoolcoolcoolcoolcoolcoolcool 		 
   
 
   
    Subject Re: safrole bomb?happy chinaman New   Reply  
    Posted by PolytheneSam (Master Searcher)  
    Posted on 07-11-01 08:23  
    Post No 189903  
   
I found a patent (US 2449644) on direct amination of stryrenes, propenylbenzenes, etc. using an amine and sodium.  Note the structure in column 2 of the patent:

Ar-CR=CH-R'

If Ar was 3,4-methylenedioxyphenyl, R was H and R' was methyl you should get MDMA.  Here's a new page I made http://www.geocities.com/dritte123/Miscpat.html which includes patents on direct amination.  Note, also, the patents on Wacker/peracid reactions.
http://www.privacy.org/article.php?sid=620&mode=thread&order=0&thold=0
http://www.privacy.org/ 		 
   

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