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

[mithyl2]

in the video novator says that around half of the 26.25g CuCl2 solution will be enough to 'cease' the black copper oxide formation.

does he actually use all of the CuCl2 solution, or only half of it?

(the last synth i did i added the CuCl2 solution in an unmeasured amount until the black copper oxide forms at the bottom of the reaction mix. i have yet to determine the quality and yield of the final product).

 

[Gordon Ramsay]

in the video novator says that around half of the 26.25g CuCl2 solution will be enough to 'cease' the black copper oxide formation.

does he actually use all of the CuCl2 solution, or only half of it?

(the last synth i did i added the CuCl2 solution in an unmeasured amount until the black copper oxide forms at the bottom of the reaction mix. i have yet to determine the quality and yield of the final product).

mithyl2I think it was not fully stated if 100% or 50% was used int he video. I think maybe 100% but it was highlighted that it might be enough to stop after 50% of the solution.
You will learn to see when the point has been reached to stop according to how your RM behaves. Yet I use almost most if not just all of it
Copper residues should not be left inside of the final product anyway

 

[mithyl2]

I think it was not fully stated if 100% or 50% was used int he video. I think maybe 100% but it was highlighted that it might be enough to stop after 50% of the solution.
You will learn to see when the point has been reached to stop according to how your RM behaves. Yet I use almost most if not just all of it
Copper residues should not be left inside of the final product anyway

Gordon Ramsayhi gordon,

have you found any difference in the yields between either using all of it or adding only enough to get the formation of the copper oxide?
(i don't know why in the video novator uses the word 'ceased' because doesn't the copper oxide form at the bottom of the flask after adding enough of the CuCl2? or am i misunderstanding something?)

what color is your reaction when you stop adding the CuCl2 solution?

 

[Gordon Ramsay]

hi gordon,

have you found any difference in the yields between either using all of it or adding only enough to get the formation of the copper oxide?
(i don't know why in the video novator uses the word 'ceased' because doesn't the copper oxide form at the bottom of the flask after adding enough of the CuCl2? or am i misunderstanding something?)

what color is your reaction when you stop adding the CuCl2 solution?

mithyl2I have not compared yields yet nor have I payed too much attention to the colours of this stage, rather temperature but I can observe it for the next synthesis

 

[mithyl2]

I have not compared yields yet nor have I payed too much attention to the colours of this stage, rather temperature but I can observe it for the next synthesis

Gordon Ramsaygood, let me know!

i think i added a bit too much on my last synth (testing if i can reliably do it by eye based on how the solution is) and i noticed very distinct and immediate color changes. upon addition of the first drops it turns blackish grey, then after maybe 15-20 minutes of stirring and another addition of several drops it turned yellow. this was all while the temp was at around 60C. for some reason i had trouble increasing the temp to 80C. (might be my hotplate). in fact it never reached 80C, but i did stir it for about 3 1/2 hours at 62C once i finished adding the CuCl2.

 

[Gordon Ramsay]

good, let me know!

i think i added a bit too much on my last synth (testing if i can reliably do it by eye based on how the solution is) and i noticed very distinct and immediate color changes. upon addition of the first drops it turns blackish grey, then after maybe 15-20 minutes of stirring and another addition of several drops it turned yellow. this was all while the temp was at around 60C. for some reason i had trouble increasing the temp to 80C. (might be my hotplate). in fact it never reached 80C, but i did stir it for about 3 1/2 hours at 62C once i finished adding the CuCl2.

mithyl2I usually add it quite fast which means continously dripping it so that the temperature is kept in check and 80°C is not passed, you maybe also want to watch out that your RM is not expanding too heavily

Maybe if you can exchange your hotplate for a heating mantle. The loss of heat on the way from your heat source to the RM will be too much to reach that temperature fast.
What temperature did you had your hotplate set on?

 

[mithyl2]

I usually add it quite fast which means continously dripping it so that the temperature is kept in check and 80°C is not passed, you maybe also want to watch out that your RM is not expanding too heavily

Maybe if you can exchange your hotplate for a heating mantle. The loss of heat on the way from your heat source to the RM will be too much to reach that temperature fast.
What temperature did you had your hotplate set on?

Gordon Ramsayi'll be using my mantle next time because of this.

its a ceramic hotplate. at first it was set to 83C but the solution wouldn't go past 60C. and it took a long time to get there from about 50C. then i turned the hotplate to 100C, nothing changed with the solution, then set the hotplate to 120C, and still nothing changed. it's happened before with other synths.

and before heating it i wrapped the flask in foil.

 

[Gordon Ramsay]

i'll be using my mantle next time because of this.

its a ceramic hotplate. at first it was set to 83C but the solution wouldn't go past 60C. and it took a long time to get there from about 50C. then i turned the hotplate to 100C, nothing changed with the solution, then set the hotplate to 120C, and still nothing changed. it's happened before with other synths.

and before heating it i wrapped the flask in foil.

mithyl2Good, a heating mantle will help.

It is important to wrap the flask and also the lower part right above the heating plate. It can also be outside vactors like a fan or something else blowing cold air that prevent the flask from heating up to 80 °C

 

[MisterAnonymous]

Reaction scheme:

View attachment 1411 ​

Equipment and glassware:

• 50 L batch reactor with a reflux condenser, top stirrer and heating apparatus in a set-up;
• Drip funnel;
• Conventional funnel;
• Laboratory grade thermometer (up to 150 °С);
• Several buckets for 10 and 20 L;
• Measuring cylinder for 1 L;
• Vacuum source;
• Laboratory scale (1-2000 g is suitable);
• Cold water bath sours for reflux condenser;
• Nutsche filter;
• pH Indicator papers;
• 5 L x2 Beakers;
• Freezer;
• Pyrex dishes for crystallization;

Reagents:

• Isopropyl alcohol (IPA) 20 L;
• Distilled water 6.2 L;
• Sodium borohydride (NaBH4) 1739 g;
• P2NP (Phenyl-2-propanone) 1000 g;
• Copper (II) chloride (CuCl2) 105 g;
• Sodium hydroxide (NaOH) water solution 25% 8 L;
• Dry acetone 2.5 L;
• Sulfuric acid (or orthophosphoric acid);

Download Video

Amphetamine synthesis

• Novator
• Apr 4, 2023
• 53
• amphetamine amphetamine synthesis nabh4 p2np p2np synthesis phenyl-2-nitropropene video synthesis

Amphetamine synthesis via NaBH4 reductive amination from P2NP...

Synthesis:

1. A mixture of IPA and H2O 2:1 (18 liters) is added to a 50 L batch reactor.
2. Solid NaBH4 (1739 g) is added in one portion and stirrer is turned on.
3. Pure P2NP (1000 g) is added in several small portions to keep the mixture temperature below 60 °С.​

View attachment 1412
P2NP (Phenyl-2-propanone)
​

4. A solution of CuCl2 (105 g) in water (200 ml) is slowly added dropwise to keep the mixture temperature below 80 °С.​

View attachment 7557 View attachment 1413
CuCl2 and CuCl2*2H2O​

5. Thereafter, reaction is kept at 80 °C for 30 minutes with help of external heating.
6. A NaOH (8 liters 25%) water solution of is added to the reaction mixture and layers are separated.
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.
9. The amphetamine free base oil is dissolved in 2 L of dry acetone.
10. Sulfuric acid (or orthophosphoric acid) is added dropwise to reach pH 6 (with a constant stirring).
11. Then, the mixture is put into a freezer for 12 hours.
12. After crystallization procedure in the freezer, the suspension of amphetamine salt is filtered with help of nutsche filter and washed with a dry cold acetone to white color. Acetone from washing procedure can be crystallized as described at steps 11-12 (amphetamine salt quality from this solution will be lower).
The reaction yield is 60-70 %.​

GhostChemist@GhostChemist i work with 10L 4 necked round bottom flask like in the video but can you please tell me wich machine with vacuum he uses to suck the Rm into another flask I need just the same thing but can't find it anywhere
Send to me private please

 

[mithyl2]

@GhostChemist i work with 10L 4 necked round bottom flask like in the video but can you please tell me wich machine with vacuum he uses to suck the Rm into another flask I need just the same thing but can't find it anywhere
Send to me private please

MisterAnonymoussorry i'm not ghostchemist, but do you mean a vacuum pump? i think the one in the video might be a rotary vane too if that's any help

 

[Melv99]

@GhostChemist i work with 10L 4 necked round bottom flask like in the video but can you please tell me wich machine with vacuum he uses to suck the Rm into another flask I need just the same thing but can't find it anywhere
Send to me private please

MisterAnonymousLook up peristaltic pump. You can find them for super cheap or expensive depending on your needs

 

[GhostChemist]

@GhostChemist i work with 10L 4 necked round bottom flask like in the video but can you please tell me wich machine with vacuum he uses to suck the Rm into another flask I need just the same thing but can't find it anywhere
Send to me private please

MisterAnonymousHi! See attached files. Vacuum pump as example and technical scheme to suck the Rm into another flask

 

[mithyl2]

has anyone else had a much larger amount of substance precipitate at the last step?

after i did the precipitation step with phosphoric acid i had more than 4 times the amount of what should be amphetamine precipitating

 

[Gordon Ramsay]

has anyone else had a much larger amount of substance precipitate at the last step?

after i did the precipitation step with phosphoric acid i had more than 4 times the amount of what should be amphetamine precipitating

mithyl2Very interesting, I'll observe and wait for an explenation of the experts on this I have heared typical street rumors as to the fact that phosphoric acid is supposed to increase yield but I'd wonder why it would yield more and also what effect this would have on the purity of the product. Amphetamines from phosphroic acid are supposed to be a little weaker, aren't they?

 

[mithyl2]

Very interesting, I'll observe and wait for an explenation of the experts on this I have heared typical street rumors as to the fact that phosphoric acid is supposed to increase yield but I'd wonder why it would yield more and also what effect this would have on the purity of the product. Amphetamines from phosphroic acid are supposed to be a little weaker, aren't they?

Gordon Ramsayyes i think so. but i don't for a moment think that all of what i have is amphetamine. but i have no idea what else it could be..

i recently tried to do a re-crystallization with vodka using a portion of what should be amphetamine. after i heated it in the vodka, all of the amphetamine dissolved except for a few bits of sediment. then i put it in the freezer overnight and when i took it out most of it was frozen at the bottom, but there was a liquid layer on top which i filtered, and from that there was a tiny bit of white powder (which i still need to weigh.)

i also tried an acid/base extraction but at the first step when i need to dissolve it in water it just made a white paste. so i filtered that and got a white paste like substance sitting on the filter, while the water dripped down, and a very very small layer of crystals formed at the bottom of the flask.

here is a more detailed post about my problem:

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/240-yield-of-amphetamine-whats-going-on.8936/#post-43483

 

[mithyl2]

yes i think so. but i don't for a moment think that all of what i have is amphetamine. but i have no idea what else it could be..

i recently tried to do a re-crystallization with vodka using a portion of what should be amphetamine. after i heated it in the vodka, all of the amphetamine dissolved except for a few bits of sediment. then i put it in the freezer overnight and when i took it out most of it was frozen at the bottom, but there was a liquid layer on top which i filtered, and from that there was a tiny bit of white powder (which i still need to weigh.)

i also tried an acid/base extraction but at the first step when i need to dissolve it in water it just made a white paste. so i filtered that and got a white paste like substance sitting on the filter, while the water dripped down, and a very very small layer of crystals formed at the bottom of the flask.

here is a more detailed post about my problem:

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/240-yield-of-amphetamine-whats-going-on.8936/#post-43483

mithyl2small update: i've tried to do an acid /base extraction but no layer formed after i added the naoh to increase the ph to 12. i then kept adding more 50% naoh solution so it became a slightly higher ph but still no layer formed. in other words, it looks like i don't have amphetamine.

i didn't remove the ipa after the copper chloride addition. might this have something to do with the final precipitate not appearing to be amphetamine? @GhostChemist

 

[Gordon Ramsay]

yes i think so. but i don't for a moment think that all of what i have is amphetamine. but i have no idea what else it could be..

i recently tried to do a re-crystallization with vodka using a portion of what should be amphetamine. after i heated it in the vodka, all of the amphetamine dissolved except for a few bits of sediment. then i put it in the freezer overnight and when i took it out most of it was frozen at the bottom, but there was a liquid layer on top which i filtered, and from that there was a tiny bit of white powder (which i still need to weigh.)

i also tried an acid/base extraction but at the first step when i need to dissolve it in water it just made a white paste. so i filtered that and got a white paste like substance sitting on the filter, while the water dripped down, and a very very small layer of crystals formed at the bottom of the flask.

here is a more detailed post about my problem:

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/240-yield-of-amphetamine-whats-going-on.8936/#post-43483

mithyl2Where do you have your P2NP from? Are you sure it is P2NP and not it's scammy little brother?

 

[GhostChemist]

small update: i've tried to do an acid /base extraction but no layer formed after i added the naoh to increase the ph to 12. i then kept adding more 50% naoh solution so it became a slightly higher ph but still no layer formed. in other words, it looks like i don't have amphetamine.

i didn't remove the ipa after the copper chloride addition. might this have something to do with the final precipitate not appearing to be amphetamine? @GhostChemist

mithyl2I agree with mithyl2
It would be nice to see the photo of your P2NP

 

[mithyl2]

I agree with mithyl2
It would be nice to see the photo of your P2NP

GhostChemisti will try to get a photo, but it should be genuine. it had all the right characteristics.

do you think not removing the ipa could be why apparently something else precipitated?

 

[mithyl2]

Where do you have your P2NP from? Are you sure it is P2NP and not it's scammy little brother?

Gordon Ramsayit came from one of the big chinese sellers on here. but the p2np not being genuine is what i was thinking...

what chemical is the scammy little brother?

 

[OrgUnikum]

Very interesting, I'll observe and wait for an explenation of the experts on this I have heared typical street rumors as to the fact that phosphoric acid is supposed to increase yield but I'd wonder why it would yield more and also what effect this would have on the purity of the product. Amphetamines from phosphroic acid are supposed to be a little weaker, aren't they?

Gordon Ramsay1 g Amphetamine Sulfate contains 720 mg Amphetamine
1 g Amphetamine Monophosphate contains 570 mg Amphetamine
This might be an explanaition.

 

[mithyl2]

1 g Amphetamine Sulfate contains 720 mg Amphetamine
1 g Amphetamine Monophosphate contains 570 mg Amphetamine
This might be an explanaition.

OrgUnikumI think it's probably from where I contaminated the p2np with sodium bisulfite during the re-crystallization stage. (adding it to etoh while the p2np is dissolved as a way of removing specific impurities). I used far to much of it (an amount equal to the amount of p2np i had, when i think i need to use about 5%).
my p2np looks and smells as it should if it was really pure though.

i did synthesize a very small batch (my very first synthesis of amphetamine) with p2np that hadn't been potentially contaminated, and where everything else about this synthesis was the same as all of the other ones I did with the (most likely) contaminated p2np. i got a 30% yield, which would indicate a poor synthesis (i made a few mistakes as one is prone to for the first time) but otherwise more or less in line with what to expect yield wise.

 

[Alchemik]

Can I change IPA for another alcohol like methanol or ethanol? and after adding 25% NaOH solution, simply extraction freebase DCM or toluene.(without evaporating alcohol). vacuum evaporation 20L of IPA takes about 20 hours on vacuum evaporator. This is a lot of time. When using Zn/HCl reduction of nitrostyrenes (methanol, 37% HCl), you don't have to evaporate methanol after reduction. After basify 25% NaOH, just extraction freebase DCM or toluene (1 liter is enough for 350g of amine freebase). Yields: 60-70% freebase.

 

[GhostChemist]

Can I change IPA for another alcohol like methanol or ethanol? and after adding 25% NaOH solution, simply extraction freebase DCM or toluene.(without evaporating alcohol). vacuum evaporation 20L of IPA takes about 20 hours on vacuum evaporator. This is a lot of time. When using Zn/HCl reduction of nitrostyrenes (methanol, 37% HCl), you don't have to evaporate methanol after reduction. After basify 25% NaOH, just extraction freebase DCM or toluene (1 liter is enough for 350g of amine freebase). Yields: 60-70% freebase.

AlchemikOf course, it`s possible to substitute alcohols. DCM and IPA are mixing. While EtOH can be "washed out" by water.