A.-sulfat--->pikrat--->hydrochloride Why???

absinth · Wed Jun 29, 2005 5:44 pm

This is only for theorie:
In a amphetamine synthesis you reduce 1-phenyl-2-nitropropen(from benzaldehyde) with lithiumaluminiumhydride.
After this you make amphetamine sulfat,then amphetamine pikrat and leave it overnight in the refrigerator(Why?).At last you make amphetaminehydrochloride and using benzene for extracting the free pikric acid.
My question is why you`ve got to make these 3steps(sulfat,pikrat,hydrochloride)?
Why you cannot make amphetamine hydrochloride first?
Benzene is a very harmful chemical.Is it possible to change it with toluol or ethanol?
Please excuse my terrible English!
Thanks a lot for all answers Smile

joe_aldehyde · huxleys associate

why don't you look up alternative syntheses. you can make the HCl salt first if you wish. go read a chemistry book

with your knowledge i wouldn't attempt ANY synthesis

absinth · Wed Jun 29, 2005 7:02 pm

@joe:This answer wasn`t very helpful.Go and read a chemistry book Confused

Why would I ask you,if I could find this in a book.
This is a missunderstanding...I don`t want to attempt it,
I want to understand it.
I think you don`t know it,too.Do you? Wink

joe_aldehyde · huxleys associate

you would find this in a book for sure. picrates are usually made for substance identification purposes since they give characteristic melting points. don't go bitching at me or i won't tell you anything anymore. your question is stupid, sorry. if you knew anything about solvents, your second question would be even more stupid. so i assume you know nothing about organic synthesis and you should go read a chemistry book.

if you wanted to understand the matters then you would research on it rather than ask somebody else to explain the whole thing to you. people are SO lazy these days!

the alchemist · Thu Jun 30, 2005 12:10 am

Amphetamine HCl is very hygroscopic if I remember correctly. It is not suitable for administration to animals. The sulfate salt is much more stable. Dissolve amphetamine freebase in Et2O and add H2SO4 dropwise.

Yes, you can use toluene as a replacement for the more harmful benzene. When performing extractions, I prefer ethyl acetate over toluene because EtOAc boils at a lower temp and is easier to remove. It is not suitable for crystallization and either toluene or Et2O should be used at this point.

icecool · Insistent Chemist

You can also use EtOH and MeOH and Et2O and acetone.
But I don't like acetone, since it gets red with H2SO4.
You can add acetone after the amphetamine sulfate has formed to suck up more water and for impurities to dissolve in then put it in the fridge for couple of hours.
Then vacuum filtrate.
And rinse with anhydrous acetone then add more H2SO4 solution 30% in anhydrous alcoholic solvent to preticipate more amphetamine.SO4.

radio879dmt · Sun Jul 03, 2005 2:32 pm

I have the old rhodium archive saved, and there's a page for amphetamine phosphate - I noticed on the net its there but the whole bottom is cut off describing, supposedly, why the phosphate salt is better than sulfate/etc.

Supposedly, the phosphate salt of amphetamine is more active in the CNS per freebase amph. molecule compared to sulfate, less peripheral side effects etc. Why I don't know - i'm not a chemist (hm, i mean, able to make some real cool shit), but if SWIM had some amphetamine around enough to play he'd freebase it and make the phosphate salt to test this out.

SWIM actually ordered a couple 4oz bottles of phosphoric acid from some beer store online (3 bucks per bottle), just to this out with DMT orally (with maoi of course). The phosphate salt of DMT does crystallize and form a solid, and SWIM did eat it once and it *seemed* to kick in faster and *seemed* to work better for the dose I ate, but it was only one time so more experimentation is necessary.

-- The reason SWIM wanted to try this was from reading about using phosphoric acid in ayahuasca, and people's descriptions of it working better etc.

---
Can anyone verify if amphetamine phosphate DOES actually work better than a salt like sulfate? - the salt is supposed to be stable and fine (not hygroscopic) so if I was about to make amph. sulfate .. well i'd make the phosphate instead Smile

stratosphere · Sun Jul 03, 2005 5:37 pm

if a substance is taken orally i can't see what it would matter as to which salt it came from, it all just becomes cations and anions in the stomach.

absinth · Wed Jul 06, 2005 3:52 am

I try to translate the text:
You drop a solution of 9.8g (60mmol) 1-Phenyl-2-nitropropen in 150ml dry Et2O to a boiling suspension of 8gr LiAlH4 in 350mL dry Et2O since 2hours.Then reflux for two hours.You cool it down and give 150mL 1M H2SO4 to it carefully.The liquid Phase are separated.You bring it with LiCO3 to pH6.Heat it to boiling and make a Filtration with "Kieselgur".
The hot filtrat was mixted with a concentrated ethanolic solution of 13,7gr Pikric acid.Then it stay in the refrigerator over night.
The crystals are filtrated,washed with Ether and dried.
You get 19,5gr amphetamine-Pikric,mp 143-154°C.
Then you put 6M HCl to the A.-Pikric to get the HCl-Salt.The free pikricacid is extrakted by benzene.The sour solution ist cooked.At last you recrystalize from Ethylacetate.You get A.-hydrocloride.
SWIM cooked it,and it works great.But i´m sure the is a simpler way to get A.-HCl, phosphat or sulfat or whatever.Do anyone know a better way to work the A.freebase up (after reducing with LiAlH4) ???
How to destroy rest of LiAlH4?

loki · guinea pig

you don't need to make the picrate, go straight to the phosphate and recrystallise in acetone/methanol (or acetone ipa, in either case, dry)

lithium aluminum hydride is removed by adding water, must be done carefully with preferably an ice bath underneath to suck the heat out because this reaction with water is quite exothermic.

in any case, you are unlikely to find you can get LiAlH4 without being suspected of being a clandestine chemist, it's right at the top of the watched chemicals list.

and i would like to vouch for the need to read. get a copy of vogels or another general organic synthesis text and learn about the things that you don't understand, like LAH and reducing agents, about picrates, melting point determination, and stuff like recrystallisation (the hows and whys)

there's plenty of e-books on chemistry available through links from the ebooks forum on this board.

joe_aldehyde · huxleys associate

swim has tried the phosphate salt, it is certainly a great advance over the sulfate since the beneficial effects described in the aforementioned paper could be fully verified. no hangover, no neurotransmitter depletion, no nothing. just plain stimulation. dihydrogenphosphates rock. swim wonders if they have advantages over hydrochlorides made from md-something compounds.

loki · guinea pig

and methylated amphetamines in general...

i wonder what is the reason for this difference. phosphates are more common in the blood than hydrochlorides, i suppose that could be involved. having intentionally infused myself with a variety of salts (mainly NaCl and MgSO4) i can definitely attest to a difference between the two in the situation of a sudden rise in these electrolytes in the blood, magnesium sulphate was pleasant whereas sodium chloride have a hot feeling and kinda made me feel somewhat nauseous.

joe_aldehyde · huxleys associate

loki, this is probably due to sodium and chloride having distinctive functions in the basic cellular processes (e.g. chloride channels triggered by GABA), whereas magnesium and sulfate are not very common thus the body is not relying on this ions to function properly, but they can mimick the action of other bivalent ions to a certain extent.

why not start a separate thread on the topic, swim is very willing to try out more phosphate compounds. except the n-methyl analogue of phenylisopropylamine, the unsubstituted one is fun enough.

loki · guinea pig

the n methyl analog is not fun? waaaat. the non-methylated phenylisopropylamine gives me a tight feeling in my throat and chest and a vague headache feeling and actually wrecks my sleep patterns much more than the n-methyl analog (!)

yeah dmt phosphate has been given a good rating from the ayahuasca folks too. i gotta get me a bottle of phosphoric by the looks of it Wink

i personally have long wondered about such things as citrates, ascorbates and tartrates, and if i could just find them easily, succinates, maleates and fumarates.

radio879dmt · Mon Jul 11, 2005 1:18 am

^^ Yeah i'm definitely going to experiment with phosphoric acid/DMT orally more, only tried the one time and it seemed to be way more potent than usual and kicked in faster (60mg DMT). I'll have to experiment more with higher doses.