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

Saul

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I did a normal distillation, Simply to improve the color. What also succeeded.
I no longer accept advice from new users. You are here for two days, and you talk here in this topic as if you were an expert.
If you had read the topic, you would have seen the full process from A to Z
stop wasting people time with nonsense .
 

KokosDreams

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Understood!

I also figured that some tend to skip steps like DCM extraction of solids..maybe for time reasons.
Looking forward to implement all my learnings soon in my own synthesis, thanks for the chat. You'll have a DM from me
 

KokosDreams

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Man it's an open forum cmon.

Maybe it's my eyes but I see that he joined 26 days after you in May..
No reason to be unpolite
 

flask

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This forum can only work if moderators with knowledge improve certain theories
I see some mistakes here
first, ammonium carbonate is never used directly with p2p.
First, ammonium formate is made.
The ammonium formate is easily made via ammonium carbonate and formic acid. Titrate
to a nice pH of 7 and remove the water.
Only then can it be used with p2p
 

KokosDreams

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I can't wait to see the forum grow more with more and more experienced people coming around!
 

Zan444

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Listen you asked people for help and i wrote you my reply.
I literally wrote you down all the basics and what i saw from experience or why do you think the people sell yellow and clear OIL in the netherlands?
No need to accept my advice cause i will not give it too you anymore.
But i think it is obvious who has more experience from us both ;)
Just remember who was stuck with hydrolysis and thought A-OIL is N-Amphetamin.
 

workworkwork

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From wikipedia it looks easy...

In the first step, a reaction between phenylacetone and formamide, either using additional formic acid or formamide itself as a reducing agent, yields N-formylamphetamine. This intermediate is then hydrolyzed using hydrochloric acid, and subsequently basified, extracted with organic solvent, concentrated, and distilled to yield the free base.

The free base is then dissolved in an organic solvent, sulfuric acid added, and amphetamine precipitates out as the sulfate salt.
 

UWe9o12jkied91d

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It is easy, some people just like to reinvent the wheel and add their own twists with no qualification to do so instead of following a recipe on the dot.
 

workworkwork

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I found this receipe on Uncle Fester book

Amphetamine synthesis via the Leuckart reaction

The magic in the reaction is to put the phenylacetone and the formamide together a couple of
days before doing the reaction.
I part phenyl acetone and 2 parts fonnamide must stand at room temperature at least 24 hours or
more. I think one week is best. It should be shaken twice a day or more. I believe the formamide is
slowly reacting with the phenyl acetone, so the longer it stands, the better!
Maybe if the temperature is higher, it reacts faster. Some people leave it for only a day, but if
you have the time, why not let it stand for one or two weeks?
Just before I got arrested, I was measuring the pH of the mixture, and I believe that it changes
every day. With a little patience, you should be able to figure out the best length of time to let it
stand.
Warning: NEVER put the formic acid with the mixture. It will ruin everything, and you will
have to start all over.
So now you have waited for a week, and you're ready to go for it. Put your mixture in a glass
flask with boiling chips. You should use as many as possible, because you need small bubbles.
This is very important! ! With a condenser on top for refluxing, the water inside the condenser must
not be very cold, because the ammonia will block the hole in the condenser, so 30° C is a good
temperature for it. You can even let all the water out, if you don't mind the smell of ammonia.
Just before you start, you take a little bit of fonnic acid and add it to the mixture. You only
need a little bit; for instance, for a 3-liter mixture, add Scc. More won't do any hann. If you put in
too much, just heat the flask without the condenser until the temperature has gone up to 1 60- 1 65°
C, and put the condenser back on.
Now you must raise the temperature to 1 80° C, and sometimes a little bit higher, depending
on the quality of your formamide. Here they use industrial grade. I've never had any problems, as
long as it's clean.
Let the mixture ret1ux for one hour after it has reached the desired temperature. The mixture
will change from light yellow to dark yellow. If it starts to darken, then your temperature is too
high.
After one hour, let it cool down, or when it is a small batch, take a sep funnel tIlled with
water and mix it with your batch. Don't use any lye at this stage.
Now take out the oil and mix it with twice the amount of hydrochloric acid. Let it reflux for
one hour.
Now you have to separate this with lye. The best thing to do is to first let it cool down, but if
it's a small batch and a big sep funnel, you can take the risk. Also, very good shaking is needed
here.
Take the oily layer and start to distill it under maximum vacuum.
Take the distilled product and mix this with twice the amount of alcohol, methanol, acetone,
or whatever you think is best. Now take 20% H2S04 and add this slowly until the p H is 7 . If you
added too much H2S04, just bring the pH back with some lye.
Now filter out the product and let it dry. Big batches take a long time to dry, so people here
put them in a centrifuge. Take a big bedsheet, put your batch in there, and let it spin. (Be careful
with sparks and such')
time.
Instead of formamide, you can also use ammonium fonnate. You don't need formic acid here.
I ' m now trying to do the reaction with only ammonia, but I ' m still working on that one.
If you have any questions, j ust write me and ask. Keep up the good work and have a good
 

workworkwork

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And Uncle Fester also talks about add a little nickle and sodium borohydride as catalysts to increase yields.
 

Saul

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Is there one person on this forum who suck seeded and had end product A-oil ?
 

Saul

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no not true he made P2P from it .
there is no one here who did it
 

KokosDreams

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Oh okay I understand :)

Why do you not go for the NaBH4/CuCL2 route?
 

Saul

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hello sir I already have P2P
this is not the problem
 

Bartholomeus

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Do not give up @Saul, buy Ammonium Formate this time and try to react with p2p again
Then when you have n-formyl, add hcl in ratio 1:1 and boil for 2 hours, after this add naoh and the a-oil comes out

Try again and post results if it works
 

Amp master

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Everyone makes it sound impossible mate it’s very easy process and end result is 52% A oil crystal clear
 
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