One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[G.Patton]

what do you mean ?

Mystery_chemistryHe means that you have to use separatory funnel

6. 25% water solution of NaOH (8 liters) was added to reaction mixture and the phases were separated.

 

[Mystery_chemistry]

but this aqueous layer is formed during the reaction. to separate and for scrap?

 

[Mclssmxxl]

but this aqueous layer is formed during the reaction. to separate and for scrap?

Mystery_chemistryNo, 2 layers is what you want.As the aq. layer gets saturated with water soluble salts it pushes the dillute isopropanol-freebase sol. out of the aq. layer.This property of isopropanol, as opposed to the other primary OH-s, to separate from water when salts are dissolved is exactly why it’s used in so many clandestine and otherwise syntheses.
Atleast I think so, hope I’m not talkin outta my ass

 

[tucoXxX]

No, 2 layers is what you want.As the aq. layer gets saturated with water soluble salts it pushes the dillute isopropanol-freebase sol. out of the aq. layer.This property of isopropanol, as opposed to the other primary OH-s, to separate from water when salts are dissolved is exactly why it’s used in so many clandestine and otherwise syntheses.
Atleast I think so, hope I’m not talkin outta my ass

MclssmxxlIf I understand correctly, is the top layer a free base? yellowish oily appearance and 70% of the mixture. and the lower one is denser.

 

[Mclssmxxl]

He means that you have to use separatory funnel

G.PattonHe’s worried because it’s happening before alkali addition, but if I am not wrong it can happen before, the alkali added just brings the phenomenon to completion.

 

[ACAB]

Atleast I think so, hope I’m not talkin outta my ass

MclssmxxlIf so I will now always salting my reaction mass before extraction with NaCl then I will have more less water to remove

 

[Mclssmxxl]

If so I will now always salting my reaction mass before extraction with NaCl then I will have more less water to remove

PennywiseYes, it works great on my own experience.Brine wash organic layer after basification removes a lot of water, I’ve done so in a pinch when I didn’t have a drying agent on hand and it was enough for a decent yield, not too far off the sol. dried over a drying agent.Don’t overdo it and let it separate for a good while aswell.
Also for a solution refusing to separate after aprox. stoechiometric alkali addition a pinch of table salt does the trick to saturate the water and get a clean break.Good to know if you don’t have hydroxide solution on hand and you’re lazy to make more

 

[ACAB]

Yes, it works great on my own experience

MclssmxxlYes, I know, using this method also in separatory funnel before if I had no clearly defined separation, but i didn't know that the salt will push IPA out of water. This way I will save a lot of desiccant because I will need much less after extracting the freebase/IPA layer.

 

[Bartholomeus]

@btcboss2022 Did you maybe already made new batch bigger batch and documented it?
I am Interested in seeing your results and final yield of A oil that comes out of this reaction on let's say 1kg p2np scale

 

[btcboss2022]

@btcboss2022 Did you maybe already made new batch bigger batch and documented it?
I am Interested in seeing your results and final yield of A oil that comes out of this reaction on let's say 1kg p2np scale

ChingShihHello,

I didn't do it yet again.
Thanks.

 

[Bartholomeus]

Hello,

I didn't do it yet again.
Thanks.

btcboss2022
I tried your reaction, with 287g p2np and when the 30g of cucl2 was added all at once it was like volcano
after the eruption of fluid through the condenser and calming of my anger i putted the flask on hotplate
and let it heat for half hour, until all the cucl2 settled to bottom with some white layer

@btcboss2022 or @William Dampier how do you control the reaction to not go volcano style when adding cucl2 at once?
I tried this synthesis in 12L flask with liebig condenser, but it still wasn't enough big to stop the reaction going out of flask
How to control it?
And how large of flask-stainless reactor would one need for 1kg p2np reduction?

 

[Bartholomeus]

@btcboss2022 and @William Dampier
What color should the reaction be after the addition of cucl2 is completed and the reaction is finished?
Upper layer stays yellow and bottom(aqueous) layer is white, is this correct?
Or should both layers be transparent - white after the whole reaction is finished?

Because when I added NaOH into finished reaction the 2 layers formed, upper layer is yellow and bottom is white, is this good?
Or is yellow color of upper layer showing that there is still unreacted p2np inside of this layer?

 

[Mclssmxxl]

I tried your reaction, with 287g p2np and when the 30g of cucl2 was added all at once it was like volcano
after the eruption of fluid through the condenser and calming of my anger i putted the flask on hotplate
and let it heat for half hour, until all the cucl2 settled to bottom with some white layer

@btcboss2022 or @William Dampier how do you control the reaction to not go volcano style when adding cucl2 at once?
I tried this synthesis in 12L flask with liebig condenser, but it still wasn't enough big to stop the reaction going out of flask
How to control it?
And how large of flask-stainless reactor would one need for 1kg p2np reduction?

ChingShihRespect the procedure next time, especially if it’s the first time you’re doing itor you’re unexperienced.It says dropwise.Do you have external cooling? Ice bath works great.

 

[Mystery_chemistry]

no separation occurs after phase separation and addition of IPA to the aqueous phase.

 

[Bartholomeus]

Respect the procedure next time, especially if it’s the first time you’re doing itor you’re unexperienced.It says dropwise.Do you have external cooling? Ice bath works great.

Mclssmxxl
Thanks for answer, but i heard the most yields from this reaction were obtained when adding it at once, next time i will try to add it drop wise just to see difference
or maybe in two portions, so there will not be such big exotermic reaction
With this reaction i cooled it in water bath at times when it seemed to be to hot

@Mclssmxxl do you have experience with this reaction? in how many grams did you try this reaction and what was your yield of oil % at the end?

 

[Mclssmxxl]

Thanks for answer, but i heard the most yields from this reaction were obtained when adding it at once, next time i will try to add it drop wise just to see difference
or maybe in two portions, so there will not be such big exotermic reaction
With this reaction i cooled it in water bath at times when it seemed to be to hot

@Mclssmxxl do you have experience with this reaction? in how many grams did you try this reaction and what was your yield of oil % at the end?

ChingShihYeah but you can only reduce so much by adding all at once, you can’t expect to reduce almost 300g of raw material in one go.If you go back in the thread i think the guy that says this even says in small scale conditions, but maybe im misremembering.
I fucked around with 25g of borohydride a few years back and did it without a procedure with mixed results.Reductions are pretty simillar tho, you get the same thing adding a bunch of styrene to redal, al hg or liah, a mess

 

[Mystery_chemistry]

gentlemen, during the evaporation of IPA two layers are formed, one milky the other yellowish. freebase in the milk phase?

 

[Mystery_chemistry]

I already know that there is good in the upper part. what then in the bottom?

 

[btcboss2022]

I tried your reaction, with 287g p2np and when the 30g of cucl2 was added all at once it was like volcano
after the eruption of fluid through the condenser and calming of my anger i putted the flask on hotplate
and let it heat for half hour, until all the cucl2 settled to bottom with some white layer

@btcboss2022 or @William Dampier how do you control the reaction to not go volcano style when adding cucl2 at once?
I tried this synthesis in 12L flask with liebig condenser, but it still wasn't enough big to stop the reaction going out of flask
How to control it?
And how large of flask-stainless reactor would one need for 1kg p2np reduction?

ChingShihIf you got a vulcano adding the cucl2 if because you don't have enough solvent in the mixture possibly because in the previous steps you evaporate a lot of it, to avoid that you must do the previous steps in a flask or reactor to lose as low as possible the solvent.

 

[btcboss2022]

@btcboss2022 and @William Dampier
What color should the reaction be after the addition of cucl2 is completed and the reaction is finished?
Upper layer stays yellow and bottom(aqueous) layer is white, is this correct?
Or should both layers be transparent - white after the whole reaction is finished?

Because when I added NaOH into finished reaction the 2 layers formed, upper layer is yellow and bottom is white, is this good?
Or is yellow color of upper layer showing that there is still unreacted p2np inside of this layer?

ChingShihIn my case after adding the cucl2 the mixture turns grey black completely and after the 30 min at 80c reflux I have 2 layers top one transparent and bottom one black about the cupper. After adding NaOH the top layer is yellow-orange colour and bottom still black of course.

 

[Bartholomeus]

If you got a vulcano adding the cucl2 if because you don't have enough solvent in the mixture possibly because in the previous steps you evaporate a lot of it, to avoid that you must do the previous steps in a flask or reactor to lose as low as possible the solvent.

btcboss2022
Thanks for those answers, it helps me a lot to understand, i didn't have a lot of solvent evaporated i think because i used condenser all the time
but the temperature of the reaction was very high as it was constantly on strong reflux when i was adding the p2np in portions
then i didn't cool down the mixture and added all the cucl2 at once and it was big volcano show
thanks again for your answers, if you again make this reaction on 1kg scale please document it and post it here