Author Topic: OTC MDMA is now easy and cheap!!  (Read 32626 times)

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yellowjacket

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Re: OTC MDMA is now easy and cheap!!
« Reply #20 on: July 19, 2001, 12:31:00 AM »
One concern with this method in the past was the formation of other, non-desirable amines ("producing a scary and paranoid trip", to quote SOMM) during the amination process. Most writeups called for distilling the product after amination. Would the A/B get all the nasties out with this method?


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AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #21 on: July 19, 2001, 10:41:00 PM »
my experience has been that when using single distilled oil. the halo-safrole will come out brown. My understanding is that pure-halosafrole is clear. brown stuff goes in, brown stuff comes out. Even after a/b you will end up with brown gak instead of crystals. The freebase must be distilled in order to get crystals. I would even distill the bromo before amination, so as that the brown nasties will not eat up all my amine first before maximum yield has been reached. as well as saving un halogenated safrol from being trashed and also interfering with the reaction.

Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #22 on: July 20, 2001, 12:05:00 AM »
I didn't have problem with brown gak.  The oil did turn dark when the HBr was bubbled, however it's my experience that safrole darkens on exposure to most acids. 

The darkness effectively disappeared in the end product after an A/B was done on part of the product recovered by evap (the non a/b'd stuff looked a bit gunkie, off color). 

Also, as far as "nasties" are concerned, many sassafras oils are suprisingly pure safrole.  When I used to tinker with isomerization, it always boiled only a degree or two higher than pure safrole, which demonstrates relative purity, if not a precise measurment.


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Chromic

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Re: OTC MDMA is now easy and cheap!!
« Reply #23 on: July 20, 2001, 12:49:00 AM »
Agent smith, that just means that your sassafras has got safrole. The impurities in sassafras will boil at a higher temperature than safrole. ie if you boil the sassafras down, it will boil at 232, then at 254, 280, etc.

Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #24 on: July 20, 2001, 03:11:00 AM »
Oh... I had myself convinced that the BP would change based on dissolved crap.  Now that I think about it, I feel like an idiot for posting that.  Oops.

Regardless, gunk was not a problem with my plain old sassafras oil.


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Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #25 on: July 20, 2001, 03:20:00 AM »
I've been toying with this, but haven't found OTC sources yet.  I think they exist, but I haven't seen em:

A more effcient way to make HBr might be to brominate tetralin (tetrahydronaphthalene) instead of naphthalene.  In my procedure, the bromine must be removed from water because if water is present, then the FeBr3 catalyst will form it's hydrate and work work.  Tetralin (to the best of my knowledge) will brominate wihtout a catalyst, which means that if it's added to an aqueous bromine solution, it *might* release HBr(g). 

I haven't tried this, because I haven't located OTC tetralin.  Tetralin is a turpentine replacement and may be found in a paint store.  Also, it's the major component of "Cuprex" a trademark referring to a pest/pediculicide that was also sold as a lice shampoo of the same name.  It seems to have gone off the market, so I dunno, but if you have an easy line on tetralin, that might work better for you.


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AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #26 on: July 20, 2001, 03:38:00 AM »
I used Iodosafrole, I wonder if thats why...
did you get crystals after a/b?


BieneMaja

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Re: OTC MDMA is now easy and cheap!!
« Reply #27 on: July 20, 2001, 03:44:00 AM »
afaik the synth via tetralin also uses iron dust as a catalysator, maybe yields are a bit higher but pure Tetralin won't be available otc, so naphthalene is the way to go.


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Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #28 on: July 20, 2001, 06:26:00 AM »
Thanks for the info Biene...

That mean that nothign is to be gained by using tetralin, if it require a catalyst like you say, then the bromine canot be in solution.  Nevermind my previous post.


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BieneMaja

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Re: OTC MDMA is now easy and cheap!!
« Reply #29 on: July 20, 2001, 03:26:00 PM »
the ref i came across for HBr via tetralin uses a 2-neck rbf, in wich is tetraline and some iron dust, one neck is for an add. funnel dropping in Br2 the other one is the gas outlet, then comes the washing flask containing tetraline.. see other HBr thread. the only advantage tetralin has (maybe) is being liquid at room temp, so it is better mixable w/Br2.


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Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #30 on: July 20, 2001, 10:24:00 PM »
Yeah, fi I could have found it, I probably would have used the tetralin.  I wonder, do you think the tetralin reaction could be used at lower temps?  If so, the flask could be cooled to reduce volatility of the bromine.  Bromine vapor was a minor problem with my naphthalene experiement, which seemed to work best at room temp or above.  I had to use a trap to ctach the bromine.


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BieneMaja

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Re: OTC MDMA is now easy and cheap!!
« Reply #31 on: July 20, 2001, 11:44:00 PM »
found the ref. again. from :
Houben-Weyl. Bd.5/4 (1960), S.18.
'[..]in the beginning, Br2 was added under  cooling [waterbath] [..]when the reaction slows down [..] [the mixture] is heated in the waterbath up to 30-40°C. the washing flask filled with tetraline is used to hold bromine vapors back. the gas trap, cooled down to -60°C, holds water, tetraline and last traces of bromine back.'

at what temp did u use your HBr generator? the setup used above is easyly built up with otc lab kit. one just has to lead his HBr through a kind of 'washing flask' loaded up w/ some more crushed naphthalene placed in a styrofoam box filled with crushed ice/NaCl or whatever. should help a lot, with the advantage over tetralin that the naphtha won't go with the HBr as it's mp is far higher than t.'s one making it much less volatile. was it that what you thought about? :)


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Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #32 on: July 21, 2001, 12:09:00 AM »
No, I hadn't thought about the volatility of the tetralin.  The naphthalene reaction proceeded with sufficient speed at room temp.  I was asking if the tetralin would proceed well at lower temp, thus eliminating the need for the trap or washing.  I see that this is not the case though, so I guess naphthalene was indeed the right choice.


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superhybrid

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Re: OTC MDMA is now easy and cheap!!
« Reply #33 on: July 21, 2001, 05:06:00 AM »
After the first page I didn't bother to read more. It is known that the halogen cation can be formed in a solution with Al halides and Fe halides. Which ones are for you to figure out.

For instance Iodine can be added to the benzene ring with AlCl3 as a reagent.

Here is the reaction

Benzene + I2-----AlCl3----->[I+ +  AlCl3I- + benzene]---->

Iodo benzene + HI  and the catylyst is rejuvinated.

This may work for other halogens and the methylene dioxy phenylalkene may be halogenated.

Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #34 on: July 21, 2001, 07:26:00 AM »
I'm sorry, did your post contribute something?


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superhybrid

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Re: OTC MDMA is now easy and cheap!!
« Reply #35 on: July 21, 2001, 08:05:00 PM »
Nope I guess I didn't did I.

Taking a week to produce a reaction is just too long in a closed system also for that matter. You may need a amine such as Et3NH3 to aid in the amination process. Don't hurt your self now.

What do we have here. I2, Br2, Cl2, F2. Which is more reactive or better yet which is more likely to come of the alkane in the amination procedure leaving the bare electophile to be snagged by the AMINE.


Agent_Smith

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Re: OTC MDMA is now easy and cheap!!
« Reply #36 on: July 21, 2001, 08:54:00 PM »
In terms of the halogens themselves, I believe fluorine (and HF) is the most reactive.  However, in terms of the halogenation reactions, there seems to be a good portion of the Hive that insists iodine is more reactive than bromine.  I really don't know, I would have thought based on periodic trends that bromine is the more reactive...?

Either way, I used bromine since it's easier to obtain from 1lb bottles of NaBr (if I did it again I'd extract the bromine form the water into DCM and then form the catalyst in the DCM bromine mix) than iodine is to obtain from lots of bottles of tincture ($$).  Also, the bromine was liquid so it reacted easier with the solid naphthalene.  If using tetralin, then solid iodine would probably be fine, however making a catalyst for that reaction would SUCK since throwing some iron into a stack of iodine crystals is idiotic.  I think bromine is the way to go.

Chlorine is an option but I haven't done any experiments with it.  There are less references for chlorinations than brominations, but from what I understand a surfacant will be required when gassing with HCl (why?).  Aminator's technique for recovering quat. surfacants form dryer sheets might work for chlorination by gassing with HCl (although I suppose doing so will require distillation later on, the synth as is will probably end in gunk if the surfacants are not removed by distillation).


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improv_chem

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Re: OTC MDMA is now easy and cheap!!
« Reply #37 on: July 21, 2001, 11:01:00 PM »
I reciently found a source of iodine that is a 10.5% tincture which should give ~50g or more of solid Iodine for about $10.  Sure beats emptying out those tiny tincture bottles and makes Iodine a practical alternative.  I think the best way to extract it is to add NaOH solution with shaking until the iodine color goes away and then boil off the alcohol and water and whatever else until you have impure NaI.  Dissolve this in a minimium amount of water and vaccume filter off the insoluable crap to get a fairly pure solution of NaI.  You then just have to add some peroxide and HCl and you have your iodine.  Wash the  stuff with distilled water a few times and then do the usual methods to dry the iodine.  Anyways... The reason i brought this up was thinking about forming HI gas using I2 and red phosphorous from match strikers.  If one was to modify Iudexk's setup for OTC MMDA on rhodium's site to fill several ballons full of HI(g) and then slowly run the gas into the drying tube, then the suckback bottle, then into the Parsley leaf oil(or safrole or whatever) through a glass tube in a graduated cylinder (narrow and tall for max absorbtion).  You could also put some fiberglass wool over the end of the glass tube to increase absorbtion.  This really isn't new but mabe you could get away with using close to molar ratio's of HI and safrole if you could slowly release the gas from the balloons with a small plastic valve like those used for fish aquariums. 
The suckback bottle might not even be necessary if you already had the HI under slight pressure in the ballons....
Just something to think about....
BTW:  great write up Agent Smith! 
this one is getting copied and pasted in case the hive ever dissappears again!!
:) -improv


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AMINATOR

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Re: OTC MDMA is now easy and cheap!!
« Reply #38 on: July 22, 2001, 10:21:00 PM »
Agent smith, you are right, the flourine is the most reactive of the halogens and would probably hold onto safrole very tightly...what we want is a halogen that is not as strong, so as it will more easily leave the safrole in exchange for the amine.

superhybrid

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Re: OTC MDMA is now easy and cheap!!
« Reply #39 on: July 22, 2001, 11:03:00 PM »
Yeah ahem so which would it be then, Cl, Br or last but not least I. Hmmmmmmm.......