PNP's into amphetamines reduction on alu foil

brain · Linguist Extraordinaire

off course its good idea, but i add in tat pieces-that when i see crystals are dissolving in solution-i throw it - because it contains wery lilte amine. and if i add to much h2so4 when the amine is in larger amount in solution-i basyfy it - destill (steam) and re precipiting.

icecool · Insistent Chemist

Okay, well I was wondering about one thing.
MgSO4 reacts with the amine.
Does it already form amphetaminesulfate?
Since it seems like there are more crystals in the solution than of what I added MgSO4.
Only a bit MgSO4 1/3 of the beaker is now full of white crystals that don't look like MgSO4...

brain · Linguist Extraordinaire

MgSO4 will react - but weeery litle !! it only reacts if it will be dissolwed in water !! [and in ether+acetone] is wery litle water, you can also dry it in exicator.

icecool · Insistent Chemist

Okay well the method worked really well.
One thing that SWIM learned when saving freebase for if you add too much H2SO4 make sure when the freebase is dissolved in ether or so, that the plastic little beaker you're saving the freebase in won't be dissolved by the ether. Rolling Eyes

Luckely SWIM noticed it before adding too much H2SO4.
Could anyone explain how to recrystalize amphetamine sulfate though?
And are the acetate and phospate and carbonate less active then the sulfate or what are the differences?
Is it possible to make amphetamine nitrate?

brain · Linguist Extraordinaire

i dont know, can it be recrystalized from H2O? (hydrolisys)

i recrystalized sulphate from solution : 10 parts of H2O, 500 parts of EtOH 90<x<91%v/v-FPIII (95 676 parts EtOH and 324 parts H2O )

icecool · Insistent Chemist

Could you be a bit more precise on what you mean?
You used 10 ml H2O and 500ml EtOH and dissolved as much amphetamine sulfate in there as possible?
What do you mean with 90>x>91% v/v FPIII (95 675 parts EtOH and 342 parts H2O)?

brain · Linguist Extraordinaire

i took it from old farmaceutic book (FP - is polish farmaceutic standard)

- 10ml H2O+500ml EtOH (this etoh-has from 90-91% of EtOH - this etoh solution was wery popular-as agent to wash skin befeore take 'syringe in body') -> the % concentration will be lower...

90<x<91% -> concentration is not bigger than 91% and no lower than 90% [it was fpIII standard-spirit]

-I cant find - how much amphetamine sulphate can be dissolwed in this solution

brain · Linguist Extraordinaire

Can I use for this reduction solution of salicyl acid in EtOH (whih is heap in my country-used in pharmacy-i just dont hawe time to separate these two things from solution - adding NaOH and destill) ??

IndoleAmine · Dreamreader Deluxe

Also the more common european pharmaceutic standards ÖAB and DAB list EtOH as 91% aequ.concentration called "weingesit", but solubility?

(about salicylic: no you cant, of course. Stop being lazy, and neutrlize with base and redistill before use!)

brain · Linguist Extraordinaire

30g P2NP was added to mixture of 125ml 80% AcOH+33ml IPA... mixture was warmed to 60C - then all P2NP dissolwed in it.
17g Al foil was amalgamated, and added in 2 portions to the flask, temperature was not less than 60 and not higher than 70C - by adding to the hot water bath or cold water bath... basyfied [in low temperature] - extracted with ether - H2SO4 was added.
Yeld = 0,02g~0g = 0% Sad

the P2NP was super pure-3x recrystalized

brain · Linguist Extraordinaire

oh, well, it was only 30g p2np... Smile

I just have nother cool idea,,, next time i will use for ekstraction - only ether ! then to ethen i will add H2SO4,,, separate the precipate, add to ethet NaHCO3+MgSO4[for drying]... to kill acid,, filtrate ether-and use it again!

-or when you add acetone, just wash ether with H2O ...

brain · Linguist Extraordinaire

[sory for that much posts-but i cant edit my mesages:?: why? ]

I just can tell you, that when i was warming it - 60-70C, when i add Al-Hg, the solution slowly become brown!! then dark gray-brown!!
-when the temp was low (30C) the solution was slowly becoming gray!

i read about 2CH from indolamine Smile

he get better yelds when he keept temp. 60-80C ... but in this case-it isnt good-i thik...

someone held that high temp? in thes reaction?

icecool · Insistent Chemist

Got a question about steam distilling.
SWIM distilled off all the solvent and then basified the mixture with Al/Hg and it was quite a thick mess though because no solvent was there so SWIM added some water to keep it stirrable.
Anyway after basifying the whole mixture the mixture turned brown/black and just after basyfieng the amine floated on top as a nice clearless slightly yellow oil and after adding more and more NaOH solution and heating it to steam distill it.
The oil became dark brown/black/red.
How come swim's pure amine oil started to get poluted?
Next time SWIM won't steam distill anymore he has got much better results with extracting with ether, or any other non polar solvent.

Another thing, one time SWIM got really nice water like colorless amine oil, but most of the time the oil is red or orange or brown/black...
What makes the difference between this?

IndoleAmine · Dreamreader Deluxe

You didn't start distillation because the floating oil turned brownish - did I get that right?

Maybe you should try to bring the pH just up to 14-15 (not to create a 50% saturated NaOH solution!!), and if things become too thick, you could always add water.....

One thought: maybe your freebase is SEEMINGLY pure if your extract directly, but nevertheless contains some unwanted substances/impurities which turn brown and ugly when heated with concentrated hydroxide solutions? Amph freebase can even be dried by letting it sit over solid KOH pellets overnight, followed by vacuum distillation directly from the flask used for drying (still containing the pellets), so I doubt that you can destroy your amine with NaOH.....

About the reason why it sometimes gives cleaner product and sometimes crap: well - finding out why is what its is all about, and you're the experimenter here... Wink

cheers

i_a

icecool · Insistent Chemist

Yeah you're right Smile

It is just what you prefer as an individual not what other people tell you what is better you should do what you like the most. Cool