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

[Curiousonion]

Almost all exothermic reactions are delayed and build up. You have to be very careful and patient

 

[WinterDust]

During step 3 and 4 when pouring in the P2nP and CuCl2.

Does the reaction heating have any special function for the synthesis that it needs to be just below 60c and 80c or can it be cooled down to 20-30c during this process in a cold bath until the exothermic reaction stops.

And when step 5 begins use external heating to keep the reaction at 80c.

Best Regards

 

[tucoXxX]

dear Members. is this amount really necessary? (Sodium borohydride (NaBH4) 1739 g
can anyone help/recommend a source where I can buy it in larger quantities but safely? Unfortunately, it is controlled in my country, so it is difficult for me to access it

 

[G.Patton]

dear Members. is this amount really necessary? (Sodium borohydride (NaBH4) 1739 g

tucoXxXYes, it is.

 

[KokosDreams]

So, I started my first synthesis today, did not go very well.

The reaction at higher volumes is VERY exothermic (200g P2nP) and just as previous poster stated, it's a very delayed reaction.

I used a 10l roundbottomflask with a 400mm cooler, unfortunetly I added too much P2nP at once (100G) and the cooler broke of accidently, so I had a 1m (3foot) volcano in my house ..

Well, spent 2 hours cleaning everything when everything calmed down and I ventilated the whole room.

So lesson, there is a delayed reaction when adding the P2nP so poor very gently and wait, secondly be vary of a good chilled cooler connected.

I'll do my second attempt tomorrow or the day after.

I'll keep people posted, best regards.

eyelow
Thanks for sharing, That's interesting tho, what's your recommended ratio of adding P2NP to the reaction?

 

[WinterDust]

Thanks for sharing, That's interesting tho, what's your recommended ratio of adding P2NP to the reaction?

KokosDreamsHi Koko,

I do not know yet, depends on if I get my previous question answered.

If I can cool the whole flask to a degree of 20-30c without loosing the purpose of the reaction then I will be able to add more at a time at a more frequent phase.

If I can't then I'll start out with a spoon full at a time and keep track of the reaction and heat development.

I will do my second attempt today or tomorrow and give a new update.

Best Regards

 

[MadHatter]

So sorry to hear that. But really, why do people make their first synthesis with such large batches? Do a couple of trial runs with 10-20 g:s of P2NP, using slow and controlled addition of every reagent first! It's a learning process and the raw material is costly. This is cookery, and you need to find the right touch and understand how reagents work before you start cooking in large vats. Easy does it.

 

[KokosDreams]

Hi Koko,

I do not know yet, depends on if I get my previous question answered.

If I can cool the whole flask to a degree of 20-30c without loosing the purpose of the reaction then I will be able to add more at a time at a more frequent phase.

If I can't then I'll start out with a spoon full at a time and keep track of the reaction and heat development.

I will do my second attempt today or tomorrow and give a new update.

Best Regards

eyelow
Gotcha!
I think you'd require a cold waterbath or a selfmade cooling system to prevent the reaction from getting out of hand.

Keep us posted and good luck!

 

[KokosDreams]

So sorry to hear that. But really, why do people make their first synthesis with such large batches? Do a couple of trial runs with 10-20 g:s of P2NP, using slow and controlled addition of every reagent first! It's a learning process and the raw material is costly. This is cookery, and you need to find the right touch and understand how reagents work before you start cooking in large vats. Easy does it.

DocX
What would be your best advice when working with larger amounts of P2NP (1kg+) to not spoil the reaction?

Cincerly,

Koko

 

[Curiousonion]

Hi Koko,

I do not know yet, depends on if I get my previous question answered.

If I can cool the whole flask to a degree of 20-30c without loosing the purpose of the reaction then I will be able to add more at a time at a more frequent phase.

If I can't then I'll start out with a spoon full at a time and keep track of the reaction and heat development.

I will do my second attempt today or tomorrow and give a new update.

Best Regards

eyelowIf you want to cool it after you add the sodium borohydride do not, it reduces its efficiency.

 

[WinterDust]

If you want to cool it after you add the sodium borohydride do not, it reduces its efficiency.

CuriousonionIt is not the Sodium Borohydride that's the "problem" it's the addition of P2nP. That's when the real exothermic reaction starts, the Sodium reaction is very mild in my opinion.

I actually thought of just buying a small freezer or refrigerator that keeps +8c and put the flask inside of it with a lever so I can manually regulate the flask from the inside, and controll the temperature through it.

 

[Curiousonion]

If you chill a reaction once the sodium is present it affects the efficiency of the sodium borohydride

 

[WinterDust]

If you chill a reaction once the sodium is present it affects the efficiency of the sodium borohydride

Curiousonion
Then, doing this reaction in larger batches without the possibility of cooling makes it quites useless?

When you say that it affects it's effeciency, do you say the reaction overall or the yield or both?

Because keeping the reaction under 60c and wanting to pout 200g P2nP that would probably takes 2-3 hours if not more if a cooling option is not available to keep the reaction atleast at 50c.

 

[Curiousonion]

It would affect the yield, sodium borohydride creates an exothermic reaction and that's how it works.
You could try to keep it steady at around 60c while you add the p2np but it could be quite hard.

 

[ElementalEnigma]

It would affect the yield, sodium borohydride creates an exothermic reaction and that's how it works.
You could try to keep it steady at around 60c while you add the p2np but it could be quite hard.

CuriousonionI was thinking maybe dissolving the starting material in IPA and slowly drip it into the reaction vessel using a SEP funnel. You recon that would affect it negatively in any way?

 

[WinterDust]

It would affect the yield, sodium borohydride creates an exothermic reaction and that's how it works.
You could try to keep it steady at around 60c while you add the p2np but it could be quite hard.

CuriousonionThank you,

This is what I mean, the P2nP reacts with the Sodium Borohydride and creates and very exothermic reaction in the flask.

So it has to be able to be cooled and semi-controlled just under 60c, that won't cause loose in yield, and higher efficiency.

I will keep you posted with my trials.

 

[Curiousonion]

yes, unfortunately it's an exothermic reaction and if you cool it while you adding the p2np it won't work. Patience is key with this.
it's also why it takes 30 minutes once the p2np is completely added for the reaction to finish.

 

[MadHatter]

What would be your best advice when working with larger amounts of P2NP (1kg+) to not spoil the reaction?

Cincerly,

Koko

KokosDreamsLike I wrote, to first do trial runs with smaller amounts to get the feel of the reaction. Otherwise to slowly add the reagents with temperature control. Basic stuff. Exothermic reactions always run the risk of getting out of hand if you're not patient.

 

[Mystery_chemistry]

So, I started my first synthesis today, did not go very well.

The reaction at higher volumes is VERY exothermic (200g P2nP) and just as previous poster stated, it's a very delayed reaction.

I used a 10l roundbottomflask with a 400mm cooler, unfortunetly I added too much P2nP at once (100G) and the cooler broke of accidently, so I had a 1m (3foot) volcano in my house ..

Well, spent 2 hours cleaning everything when everything calmed down and I ventilated the whole room.

So lesson, there is a delayed reaction when adding the P2nP so poor very gently and wait, secondly be vary of a good chilled cooler connected.

I'll do my second attempt tomorrow or the day after.

I'll keep people posted, best regards.

eyelowon a 10l flask at ease you will carry out a reaction with a loading of 250g p2np. there is one condition. you need to keep the flask cool when adding p2e.g. about halfway through the addition the reaction will stabilize and you can refine your p2np faster

 

[Mystery_chemistry]

Hi Koko,

I do not know yet, depends on if I get my previous question answered.

If I can cool the whole flask to a degree of 20-30c without loosing the purpose of the reaction then I will be able to add more at a time at a more frequent phase.

If I can't then I'll start out with a spoon full at a time and keep track of the reaction and heat development.

I will do my second attempt today or tomorrow and give a new update.

Best Regards

eyelowthe first stage, i.e. adding p2np, is to be kept at a low temperature ... when you add cucl2 mix well and turn on the heating ...

 

[Curiousonion]

the first stage, i.e. adding p2np, is to be kept at a low temperature ... when you add cucl2 mix well and turn on the heating ...

Mystery_chemistryInteresting, I read on a synthesis paper that low temp can lower the yield.
How low would you recommend? Cause if it can go below zero then the addition could be done extra fast