Need help convert bmk 5449-12-7 to free base A-oil

UWe9o12jkied91d

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I think what is reffered to as a-oil is amphetamine freebase dilluted with methanol
 

serialz

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For me the A-Oil is :

Here

I hate this langage.

It would be easier if people talked about molecules and not about a language coming from the street...
 

UWe9o12jkied91d

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I know, much better to talk about molecule, I was just trying to not make an already confused guy even more confused
 

Saul

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dear serialz you should not feel attacked.
the earlier explanation about the calculation of the Mols was phenomenal.
you explained in detail there what I had to do to convert my P2P to N-formylamphetamine.

yesterday I just asked a question and suddenly you add an whole explanation.
sorry but i found this very strange. because you already explained everything from P2P to N-Formylamphetamine .
now suddenly toluene and hydrochloric acid were added.
sorry but this was very confusing for me. and still is actually
So forgive me if I seem rude to you.

I don't want amphetamine at all
i want freebase amphetamine N-Formylamphetamine and yes street name in europe A-oil .

so now i ask do i need that extra step of toluene and hydrochloric acid ?

and the real question I wanna to ask
you calculate 8 moles of formic acid ( 433gr )
excess means overtollig So actually it's not wrong to add too much formic acid? because I personally think that I have used too little formic acid and that is why after a total time of 12 hours of cooking that suddenly a discoloration took place .
formic acid is not expensive at all I prefer to use enough so iam safe .
is this allowed?
 
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Saul

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PS: I'm in a learning phase that's why I work with only 100ml quantities off P2P
so it's not a loss if it fails. that's just part of it
 

Saul

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hello my friend

I need some help plz
i'm done cooking
this time it worked out very well.
after 14 hours of cooking without interruption and with a very powerful mixer I have a nice thick yellow top layer in my flask.
so now i would like to start on the last stage . the ph off the top and bottom layer is ph04
Do I have to separate these already? so now i have to raise the ph with hydrochloric acid to ph11
the washing with tolueen how do they do this ?
 

UWe9o12jkied91d

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separate, then add toluene to water layer, mix, separate again, repeat 1-2 times ->HCl -> dry - >precipitate with h2so4
 

Saul

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I try to like your post, but it is not working

Thank you for your answer.

They also say to me that I needed NaOH for the last step ?
And after add HCI I must again heat for 3 hours, reflux ?
is this correct ?
 
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UWe9o12jkied91d

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This the procedure, did you do anything different? except vaccum ofc

1. A solution of 1-phenyl-2-propanone (0,827 g, 6.2 mmol) and formamide (3,5 ml) was heated at 160-170 *C for 16 h.
2. The mixture was cooled to room temperature, and 30% hydrogen peroxide (5 ml) was added.
3. After stirring for 15 min, the reaction mixture was extracted with benzene (2x25 ml), and the combined benzene extracts were evaporated under reduced pressure to yield a dark oil.
4. The oil was dissolved in a solution of methanol (5 ml) and 15% HCl (5 ml) and stirred at reflux for 2 h.
5. The reaction mixture was evaporated under reduced pressure. The remaining product was dissolved in water (25 ml) and washed with methylene chloride (2x20 ml).
6. The aqueous solution was then made basic (pH 10) by the addition of NaOH pellets and extracted with methylene chloride (2x25 ml).
7. The combined methylene chloride extracts were evaporated to yield the product amine as a yellow oil
 

Saul

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Yes everything.

I follow the PDF file here in this topic, but the last step is not included. and I only need the last step .
I have now N-formylamphetamine liquid ph4 and I want freebase liquid ph11
 

UWe9o12jkied91d

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you are on step 3 of the procedure

4. The oil was dissolved in a solution of methanol (5 ml) and 15% HCl (5 ml) and stirred at reflux for 2 h.
5. The reaction mixture was evaporated under reduced pressure. The remaining product was dissolved in water (25 ml) and washed with methylene chloride (2x20 ml). for now its not necesary to vaccum, just use your extracted organic layer(oil).You cant add naoh to just oil + solvent so you need some water, add naoh, extract your regular amphetamine freebase, precipitate.
 

Saul

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question for serialz.

After the 24h reflux, just let everything in the flask ? And start with HCI treatment ? Or separate the two layers first
before starting the treatment ?
How does washing with toluene work ?
 

UWe9o12jkied91d

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The initial reaction mass is separated and you work with the extracted oil and the following washings pooled together.Notice please how the procedure reffers to what is being treated with HCl as oil.
Washing can be meant as extracting.For example after separating you add more toluene to water layer, shake well, wait to separate, put in funnel, separate.Another thing that can be meant is say you have a glass with freebase in it, you pour it off somewhere else, but there is still material on the glass, you add toluene, "washing" the glass of any remains of product.
 

Saul

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How much HCI I mix with the top layer, let's say it is 300 ml

I realy dont get it that HCI will increase the ph becouse it have ph 1
 

UWe9o12jkied91d

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you add the hcl to turn your n-formyl into just regular amp. base.Also HCl will decrease your pH, not raise it.In the procedure for 0.8-0.9 p2p 5ml of 15% HCl are used, try an equivalent amount I suppose.
 

Saul

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so how do I get it afterwards to ph 11 ?
 

UWe9o12jkied91d

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6. The aqueous solution was then made basic (pH 10) by the addition of NaOH pellets and extracted with methylene chloride (2x25 ml).

After HCl you have a 2 layer reaction mass, you add sodium hydroxide to that, separate, extract with toluene or whatever you have, pool extracts, dry with mgso4, precipitate.
 

Saul

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can I use also tolueen for this becouse I dont have methylene chloride ?
 

melk

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Hello to all members
I am new here.
I have a question off this synthesis
is there a way from N-formylamphetamine. To normal speed ( paste )
Because I don't want unstable oil
I want the best quality possible with the things I have, and I think that oil is not the answer
who can help me ?
 

UWe9o12jkied91d

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yes, any non-polar works xylene, pet ether, cyclohexane, benzene, ipa too if your aq layer is basic or brine saturated, acetates hurt yield not worth using
This is what we are talking about in this thread.Formetorex is obtained by leuckart amination followed by hydrolysis with HCl yielding amphetamine freebase, which can keep for months dilluted and kept cold.
 
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