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

[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.

 

[tucoXxX]

this would be the aqueous layer. I added 25% naoh solution. which layer do i need ?? I was a little confused

 

[Marvin "Popcorn" Sutton]

this would be the aqueous layer. I added 25% naoh solution. which layer do i need ?? I was a little confused

tucoXxXWrite down what proportions of reagents you used.
How long does the mixture stand after adding the NaOH solution in the photo?

 

[w2x3f5]

Hello. 10L IPA
Distilled water 3.1 L;
Sodium borohydride (NaBH4) 870 g;
P2NP (Phenyl-2-propanone) 500 g;
Copper (II) chloride (CuCl2) 52 g.
Sodium hydroxide (NaOH) water solution 25% 4 L;. these reagents . this was the bottom layer (water layer). I added Ipa these layers are formed. I let it rest for 10 minutes

tucoXxXif the alkaline amine goes into the upper alcohol layer. if ph is acidic, it will be in the lower layer in the form of a dissolved salt. In any case, there will be losses with this method of allocation.

 

[tucoXxX]

Write down what proportions of reagents you used.
How long does the mixture stand after adding the NaOH solution in the photo?

Marvin "Popcorn" Suttonabout 2 minutes and two layers are formed, I leave it alone for 30 minutes.

1754g nabh4
1000g p2np
100g cucl2

 

[mithyl2]

is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?

 

[ACAB]

is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?

mithyl2For best results use overhead steering for flask.

 

[mithyl2]

For best results use overhead steering for flask.

ACABand i was hoping to be able to use the magnetic stirrer lol. but i had my doubts about whether it would be strong enough.

 

[ACAB]

and i was hoping to be able to use the magnetic stirrer lol. but i had my doubts about whether it would be strong enough.

mithyl2It could take 6 hour, take time for synthesis, take attention with temperature.

It depends on how much aluminum is in the flask and how good your magnetic stirrer is.
Overhead stirrers have more power.

 

[tucoXxX]

I don't think you should do anything with the IPA/base after the election. there is too much alcohol in it, I would like to reduce the ipa. I think the quality of the oil may be poor due to too much IPA.

 

[WinterDust]

I don't think you should do anything with the IPA/base after the election. there is too much alcohol in it, I would like to reduce the ipa. I think the quality of the oil may be poor due to too much IPA.

tucoXxXYou are wrong.

 

[tucoXxX]

I messed up the kayak. I cleaned the mixture on the filter and threw away the insoluble precipitate. I poured it back into a reactor.

I added a 25% NaOH solution. two layers formed. I rest for half an hour. upper yellow layer (Ipa/base). bottom layer transparent (water layer).

I drop the aqueous layer into a flask. I add Ipa, layers are formed. I rest for half an hour.

the top layer is transparent (base/Ipa) is what I need. I put the base extracted from the aqueous layer into the rotary evaporator. The cooling is 8 degrees, the vacuum is on, the temperature of the bath is 80 degrees, the ipa starts to evaporate here.

I pour Ipa vaporizer base into a glass. what should i do with this foundation (transparent)?? what will happen if I pour it into Ipa/ base mixture?? why do you have to do this?

and the yellow layer (base/Ipa) into the reactor. 3 liters of IPA/base mixture. how can i reduce ipa??? is this also rotovap? because if I start to evaporate in the reactor at 80 degrees, the Ipa drips out of the condenser. my problem with this is that it ends up being red and the smell goes away. I think I messed up.

 

[panchaspsycho]

I messed up the kayak. I cleaned the mixture on the filter and threw away the insoluble precipitate. I poured it back into a reactor.

I added a 25% NaOH solution. two layers formed. I rest for half an hour. upper yellow layer (Ipa/base). bottom layer transparent (water layer).

I drop the aqueous layer into a flask. I add Ipa, layers are formed. I rest for half an hour.

the top layer is transparent (base/Ipa) is what I need. I put the base extracted from the aqueous layer into the rotary evaporator. The cooling is 8 degrees, the vacuum is on, the temperature of the bath is 80 degrees, the ipa starts to evaporate here.

I pour Ipa vaporizer base into a glass. what should i do with this foundation (transparent)?? what will happen if I pour it into Ipa/ base mixture?? why do you have to do this?

and the yellow layer (base/Ipa) into the reactor. 3 liters of IPA/base mixture. how can i reduce ipa??? is this also rotovap? because if I start to evaporate in the reactor at 80 degrees, the Ipa drips out of the condenser. my problem with this is that it ends up being red and the smell goes away. I think I messed up.

tucoXxXWhy did you evap the IPA, follow the video. Do it again with steps in video IPA doesn't mess up the amphetamine it just makes it smelly lol.

 

[panchaspsycho]

I messed up the kayak. I cleaned the mixture on the filter and threw away the insoluble precipitate. I poured it back into a reactor.

I added a 25% NaOH solution. two layers formed. I rest for half an hour. upper yellow layer (Ipa/base). bottom layer transparent (water layer).

I drop the aqueous layer into a flask. I add Ipa, layers are formed. I rest for half an hour.

the top layer is transparent (base/Ipa) is what I need. I put the base extracted from the aqueous layer into the rotary evaporator. The cooling is 8 degrees, the vacuum is on, the temperature of the bath is 80 degrees, the ipa starts to evaporate here.

I pour Ipa vaporizer base into a glass. what should i do with this foundation (transparent)?? what will happen if I pour it into Ipa/ base mixture?? why do you have to do this?

and the yellow layer (base/Ipa) into the reactor. 3 liters of IPA/base mixture. how can i reduce ipa??? is this also rotovap? because if I start to evaporate in the reactor at 80 degrees, the Ipa drips out of the condenser. my problem with this is that it ends up being red and the smell goes away. I think I messed up.

tucoXxXI have done this exact same synthesis just follow the video and after you acidify if you don't want that IPA mess/smell clean it with some acetone and leave for a week or two on fresh air and light to purify and dry.

 

[tucoXxX]

I have done this exact same synthesis just follow the video and after you acidify if you don't want that IPA mess/smell clean it with some acetone and leave for a week or two on fresh air and light to purify and dry.

panchaspsychoHello. now we managed to build a steam distillation system. with the help of a nice forum member. the distillation is currently in progress, I think I'll be done in 2 hours I'm only making a small amount now, if I succeed, I'll use 1kg p2np. I don't have the opportunity to dry it outdoors, in the fresh air, in the sunlight, I have to learn how to distill it. how much did you make and what was the yield?

 

[tucoXxX]

7. The aqueous phase is extracted with 8 liters of IPA. Amphetamine free base is dissolved in IPA and IPA layer density is changed, hence, it is separated from aqueous layer.
8. The IPA from step 7 extract is evaporated on vacuum to an amphetamine free base oil and combined with free base from step 6.

Why should it be combined with the free base? does this step bring extra income or what is the point?

 

[WinterDust]

7. The aqueous phase is extracted with 8 liters of IPA. Amphetamine free base is dissolved in IPA and IPA layer density is changed, hence, it is separated from aqueous layer.
8. The IPA from step 7 extract is evaporated on vacuum to an amphetamine free base oil and combined with free base from step 6.

Why should it be combined with the free base? does this step bring extra income or what is the point?

tucoXxXYou do 500g reactions, how do you come to the conclusion of 8l of IPA?

Why should you ad the extracted freebase to your previous freebase, is that an honest question?

 

[tucoXxX]

You do 500g reactions, how do you come to the conclusion of 8l of IPA?

Why should you ad the extracted freebase to your previous freebase, is that an honest question?

WinterDust6 liters of Ipa at the beginning of the synthesis, 4 liters for layer selection. it is not necessary to add 8 liters at the same time. I use Methanol instead of IPA, the final product will smell less of alcohol. But because of this I can't separate layers (metalon can't do it, so when it asks for alcohol for layer selection) it is necessary to add dcm. the two layers must be combined because the yield will be higher, I think. I finally managed to make the oil I wanted. The picture shows the result, before salting.

 

[fufu]

Hello experts, do you know if i can use sodium bicarbonate to get freebase in amph from p2np reaction? Thank you.

 

[tucoXxX]

7. Steps .


Which layer do I need? After adding ipa, 2 layers are formed. top layer transparent, clean, slightly oily surface. lower layer white dense jelly. it says Ipa's density changes and separates from the water layer. its density changes, could it mean that it has become a jelly and a lower layer? noob question but useful.

 

[WinterDust]

7. Steps .


Which layer do I need? After adding ipa, 2 layers are formed. top layer transparent, clean, slightly oily surface. lower layer white dense jelly. it says Ipa's density changes and separates from the water layer. its density changes, could it mean that it has become a jelly and a lower layer? noob question but useful.

tucoXxXYour question is answered by me in previous post. Go back and look, there are even pictures.

 

[tucoXxX]

thank you, it became clear. I knew which layer, but I couldn't explain to myself why that layer??

 

[tucoXxX]

thank you, it became clear. I knew which layer, but I couldn't explain to myself why that layer??

 

[tucoXxX]

thank you, it became clear. I knew which layer, but I couldn't explain to myself why that layer??

tucoXxXI'm sorry, I've messaged you several times, please delete it..

 

[chicaloca]

Hello, After the reaction I quench with dilute HCl and distill IPA off to 100°C but the next day when I come to separate the phases the flask don't stir. Theres a hue in the flask. Here is pics can someone help me to understand and telling what options I have thx

 

[WinterDust]

Hello, After the reaction I quench with dilute HCl and distill IPA off to 100°C but the next day when I come to separate the phases the flask don't stir. Theres a hue in the flask. Here is pics can someone help me to understand and telling what options I have thx

chicalocaHi,

First of all, where in the synthesis does it say that you should use HCL? Hint: Nowhere, so don't.

Second, since you distill in 100c I assume you do open distillation, don't do this, use vacuum distillation instead.

Try again and respost results.

Best regards

 

[chicaloca]

More hydroxide.
You should use a non polar such as toluene or something for extraction of the remains, even if ipa works

UWe9o12jkied91dOkay Im gonna add 25% NaOH and after what should i do? Extract with DCM?
I have some

 

[chicaloca]

Okay Im gonna add 25% NaOH and after what should i do? Extract with DCM?
I have some

chicalocaOkay I've add 25% NaOH but I don't think the bug came from NaOH because for phase separation it's all right... The problem occurs just after; when I want to extract the aquaus phase anyway, ... I add DCM but even with a NP like DCM there is NO CLEAR phases separation!,