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Author Topic: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!  (Read 777 times)

atara

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #20 on: October 24, 2010, 04:19:24 PM »
This should help:
http://dx.doi.org/10.1016/S0040-4039(00)71162-2
I have a feeling NAPQI will hydrolyse easily to benzoquinone and acetamide. Both are pretty useful.

Evilblaze

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #21 on: October 24, 2010, 05:12:51 PM »
I just have a new report from an unsuccessful synthesis. Yeah....

We just tried to make DOI by this recipe:
Quote
DOI
The glass is ground thoroughly with 1.90 g (7.36 mmol, 1 eq) nitrate, 2,5-DMA and 1.25 g (1 equiv, MW 169.9) of silver nitrate and placed in a 100 ml flask, add 20 ml of methanol, the flask wrapped in aluminum foil, stirred 10 minutes (almost everything has to be dissolved), then dropwise within 10-15 minutes there is added a solution 1.87 g (1 equiv, MW 253.Cool powdered in advance (otherwise dissolve!) iodine in 50 ml of methanol (dissolved in parts!) . The mass is stirred an additional 1 hour, light-yellow silver iodide is filtered through a fine (S4) filter, the filtrate evaporated, stir in 100 ml of warm water (still poorly soluble), made alkaline KOH solution, a brown oily base is extracted with DCM, washed with water, dried carbonate potassium, evaporated, diluted with methanol, acidified to a weakly acid reaction HCl, evaporated, co-uparivavyut with a mixture of toluene-IPA, the remainder was ground with MTB, filtered, washed with MTB, and then with acetone. Yield - 2.02 g (77%, MW 357.6 (CH)) - crystals almost pure white. Mp. - About 200OS (Literary mp. 201OS).

We just started from 3g of DOH-nitrate.
Dissolving the DOH freebase is not possible in MeOH and not even all of the AgNO3 dissolved. After this an iodine solution was added to the previously prepared DOH and AgNO3 solution and this was stirred for one hour and left to stand for another hour.
The color of the iodine still remained, but not so intensive like in the beginning.
This solution was filtered and poored on water and added some NaOH to pH 14. There was no brown oil or any kind of oil in the solution /looks bad/. This solution was extracted twice with DCM, the combined extracts were distilled and the remaining oil was kept.
The remained oil was dissolved in EtOH, some cc. H2SO4 was added but no crystals formed.

Let's wait and see what will happen yesterday with this solution, but it doesn't looks great....

director of sound

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #22 on: October 31, 2010, 11:21:41 AM »
the route from anethole seem the most economical as most of the chems used can be easily procured or made, i sourced anise oil from the same place i get my other essential oils at $40 for 950ml. toluene is easy as cake to get (atleat in the us) potassium dichromate could be used as the oxidative agent rather than sodium bichromate like the paper. DCM, formic acid and strong H2O2 can be had on ebay. chloroform can be easily made via the haloform rxn between acetone and calcium hypochlorite from pool shock (you gotta distill it as its made..). my belief is that methyl iodide could be used in place of dimethyl sulfate (which is also easily made from H2SO2 and methanol). ammonium acetate is easy to get but the nitroethane might pose a problem. mabey make from sodium ethyl sulfate and sodium nitrite but i do not know the yields for that one. or an ethyl halide and silver nitrate... i ma have to give this a whirl, gotta try to come up with an easy way to DOM/STP, DOPR (the propyl analog) could be interesting but i dont know about the 30hr trip....

hypnos

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #23 on: November 08, 2010, 09:02:06 AM »
BTW  Very nice thread  evilblaze 8) and thank you for sharing all the excellent experience you have had...sorry not saying something sooner :P

  Any bioassay results worth mentioning? :)

 
Quote
could be interesting but i dont know about the 30hr trip....
yeah.. :P :P :P :P :P :P
« Last Edit: November 08, 2010, 09:05:42 AM by hypnos »
"the two things you can give away and never lose, are what you know, and how you feel...."

Qabal

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #24 on: December 21, 2010, 01:48:50 PM »
Yes!

A friend had a book of an unspecified DOX - presumably DOB.

Duration is directly proportional to the amount taken - the difference in duration between two and three hits is different by about six hours. Another friend ingested six of these and was awake for 50 or so.

Benzodiazepines are now a must if I were to ever embark again on such a trip.

The only thing that soothed me during the entire trip was the fact that I wasn't on more DOB.

I lingered in limbo of amphetamine psychosis and true psychedelic beauty, never going anywhere  - very speedy, very tiring.

letters

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Re: DOX thead, the place for every 4 substitued 2,5 dimethoxy amphetamine!
« Reply #25 on: December 24, 2010, 03:39:42 PM »
people should stop using the old-school dean-stark/toluene nitroaldol reaction/dehydration for nitroalkenes!
It is just a wast of good chems.
There are much better procedures, using primary amines (or acetate of primary amines) as efficient catalysts. Methylamine works, ethylamine works, ethylenediamine works well.
Solvent should be alcohol, ipa/methanol/ethanol.
reflux time is no more then 1-1.5 hours.
yield are usually quite good.
That black tar you showed is just nasty.
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