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

[KokosDreams]

View attachment 1413
CuCl2​

​

William Dampier@G.Patton According to the colour of the CuCL2 I would guess it is not CuCL2, but Copper (II) Chloride Dihydrate instead.

Am I correct that this is Copper (II) Chloride Dihydrate (CuCL2 2H2O) with the CAS: 10125-13-0?

The description of my product says that regular CuCL2 has a brownish colour while the CuCL2 Dihydrate has a blue-greenish colour like shown on the picture. I am a little confused as it says CuCL2 but has the colour of CuCL2 2H2O

 

[G.Patton]

@G.Patton According to the colour of the CuCL2 I would guess it is not CuCL2, but Copper (II) Chloride Dihydrate instead.

Am I correct that this is Copper (II) Chloride Dihydrate (CuCL2 2H2O) with the CAS: 10125-13-0?

The description of my product says that regular CuCL2 has a brownish colour while the CuCL2 Dihydrate has a blue-greenish colour like shown on the picture. I am a little confused as it says CuCL2 but has the colour of CuCL2 2H2O

KokosDreamsYes, you are right. Anyway, you'll use CuCl2 with water. You can take CuCl2*2H2O and count same amount of CuCl2 there.

 

[KokosDreams]

Yes, you are right. Anyway, you'll use CuCl2 with water. You can take CuCl2*2H2O and count same amount of CuCl2 there.

G.PattonPerfect, that's what I assumed. Thanks a lot!

@Curiousonion there we go, confirmed

 

[KokosDreams]

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);

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 %.​

William DampierI love the update on the post @William Dampier

Am I correc with the assumption that I have to use a max of 50% of the reactors volume until step 4?

In a 20L Reactor, that would mean a RM of 10L, which means I can load up to

 

[G.Patton]

Am I correc with the assumption that I have to use a max of 50% of the reactors volume until step 4?

In a 20L Reactor, that would mean a RM of 10L, which means I can load up to

KokosDreamsCorrect, reactor volume have to be ~30-50% empty during reaction. It is due safety reasons.

 

[KokosDreams]

Correct, reactor volume have to be ~30-50% empty during reaction. It is due safety reasons.

G.PattonGotcha, so in a 20L reactor I can easily load approx. 475g P2NP?

50% of reactor volume before the exothermic reaction and 70% of volume during the exothermic reaction including foaming?

 

[G.Patton]

Gotcha, so in a 20L reactor I can easily load approx. 475g P2NP?

50% of reactor volume before the exothermic reaction and 70% of volume during the exothermic reaction including foaming?

KokosDreamsyes, do you mean 50 and 70% of loaded space?

 

[KokosDreams]

yes, do you mean 50 and 70% of loaded space?

G.PattonI mean 50% of loaded space so that it can expand to a maximum of 70% during the exothermic reaction, if it should fume.

My guess is that if I load 70%, it could get quite close if it expands to 90%.

What do you think?

 

[Mo0odi]

Thank you everyone for sharing the information. Soon I will join you as

 

[Mo0odi]

I am waiting for the materials and equipment to be completed

 

[Mo0odi]

Yes, you are right. Anyway, you'll use CuCl2 with water. You can take CuCl2*2H2O and count same amount of CuCl2 there.

G.PattonIs there a difference between this CuCL2 2H2O and this CuCL2 or are they the same

 

[Mo0odi]

What do you recommend to buy and can you give me the cas number

 

[KokosDreams]

What do you recommend to buy and can you give me the cas number

Mo0odiYou can simply buy:

Copper (II) Chloride Dihydrate (CuCL2 2H2O) with the CAS: 10125-13-0

It has the same effect as regular CuCL2 and costs less, the same weight/volume can be used

 

[Mo0odi]

You can simply buy:

Copper (II) Chloride Dihydrate (CuCL2 2H2O) with the CAS: 10125-13-0

It has the same effect as regular CuCL2 and costs less, the same weight/volume can be used

KokosDreamsThank you, I was so confused

 

[Mo0odi]

Cupric Chloride pure, 98%
(Copper (II) chloride)
CSA7447-39-4

These are available at I don't know if they are the same

 

[KokosDreams]

Thank you, I was so confused

Mo0odiYou are welcome!

Cupric Chloride pure, 98%
(Copper (II) chloride)
CSA7447-39-4

These are available at I don't know if they are the same

If you search more you will find the one I have written above in EU shops, unrestricted
THe CAS is different, so it is another chemical. I assume it's regular CuCL2 and not CuCL2 2H2O

 

[WinterDust]

Hi,

Question,

When the amphetamine oil is crystalized with sulfuric acid, it's time to filter out the amphetamine with a Buchner Funnel, my question is. What type of filtration paper it recommended for this?

For example, I'm looking at a filter with the following properties, is this a good recommendation?

Filter Properties:
Filter papers made of tissue paper
Hard filters - filtration time 140 seconds (Retention> 2 µm). Slow filtration.
Dense filters for fine and very fine sediments.
Weight: 85 g / m2.
Thickness: 0.17 mm.
Filtration time: 140 s.
Retention:> 2 µm.

Best Regards

 

[ASheSChem]

good question.. i'm intersted too..
actualy i use this

but i don't know what it is lol

i saw a lot of type of filter "qualitative" or "quantitative" and in each category a version "slow" "medium" and "fast"...
what's the best ?

 

[WinterDust]

BUMP!

Question,

I am currently doing the following ingredient scale:

IPA 2:1, 3,6l
NaBH4, 348g
P2nP, 200g
CuCl2, 20g + 40ml H2O
NaoH 25%, 1,6l

I learned that the scale was linear so these are the measurements I concluded.

Now to the question, if I keep all of the ingredients at the same scale but only increase the P2nP too 300g instead, what would the outcome be?

Best regards

 

[Bartholomeus]

BUMP!

Question,

I am currently doing the following ingredient scale:

IPA 2:1, 3,6l
NaBH4, 348g
P2nP, 200g
CuCl2, 20g + 40ml H2O
NaoH 25%, 1,6l

I learned that the scale was linear so these are the measurements I concluded.

Now to the question, if I keep all of the ingredients at the same scale but only increase the P2nP too 300g instead, what would the outcome be?

Best regards

eyelow
Everything has to be increased proportionally
But you can try and only raise the weight of p2np and you will see for yourself what will happen
Then you can update us here with your results so we all learn something new from it
Just keep up the work