Synthesis of Amphetamine from P2NP via SnCl2 and Zn

[TucoSalamanca.]

what can be used instead of magnesium sulphate

 

[mithyl2]

what can be used instead of magnesium sulphate

TucoSalamanca.magnesium sulfate is very easy to get worldwide I think. Are you having problems getting it?

and you need to make it completely dry before using it. I put mine in a microwave.

 

[yuiopjkl]

what can be used instead of magnesium sulphate

TucoSalamanca.Sodium sulfate anhydrous. Na2SO4

 

[GDC]

Same problem here...
After Zinc and Hydroxidation yellow stuff on top and after addition of DCM:
Clean solution on top (PH7 on a scale of 14) and Milky stuff on the bottom (PH 11)...
But on your pics it is different..

Which route you use? Propene to Oxime by SnCl2/HCl and then?

different routes starting from nitropropenes , Hive Methods Discourse

Best regards

 

[GDC]

Same problem here...
After Zinc and Hydroxidation yellow stuff on top and after addition of DCM:
Clean solution on top (PH7 on a scale of 14) and Milky stuff on the bottom (PH 11)...
But on your pics it is different..

Which route you use? Propene to Oxime by SnCl2/HCl and then?

different routes starting from nitropropenes , Hive Methods Discourse

Best regards

GDCI'm not sure about the timing... GAA -> Zinc -> NaOH ?? Max. Temperature ??

Step	Equipment	Chemicals
1. PREPARE;	Beaker 100ml	15g P2NP; 50ml Acetone
2. PREPARE;	Beaker 500ml	NaOH, H2O 1:1 Solution (200g;200ml)
3. PREPARE;	Beaker 150ml	NaOH, H2O 1:2 Solution (50g;100ml)
4. PREPARE;	Flask 250ml, Temperature Sensor, Reflux Condenser	50ml Acetone; 42g SnCl2; P2NP Solution;
5. ADD;		50ml Acetone; 42g SnCl2;
6. ADD;		P2NP Solution;
7. WORK; 20 Min.	Stirrer
8. PREPARE;	Beaker 150ml;	HCl Solution (150ml H2O; 4ml HCl
9. ADD; To Flask		HCl Solution
10. PREPARE;	Beaker 1000ml
11. ADD;		Transfer Mixture to Beaker
12. ADD;		400ml NaOH Prepared 1:1 Solution; !PH11!
13. PREPARE;	500ml Beaker, Buchner, Erlenmeyer, Syringe	Ethyl Acetate,MgSO4
14. EXTRACT;	Stirrer, Syringe	3x50ml Ethyl Acetate
15. DRY;		MgSO4
16. FILTRATE;	Erlenmeyer, Buchner
17. PREPARE;	500ml Flask, Stirrer	60ml GAA, 10g Zinc
18. ADD;		60ml GAA
19. ADD;		Mixtue of Oxime
20. ADD;		10g Zinc
21. WORK; 15 Min.	Stirrer
22. PREPARE	Buchner, Erlenmeyer
22. ADD;		150ml NaOH Prepared 1:2 Solution; !PH11!
23. FILTRATE;	Erlenmeyer, Buchner
24. PREPARE;	500ml Beaker, Buchner, Erlenmeyer	50ml DCM
25. ADD;	Filtrated Mixture
26. ADD;		50ml DCM
27. PREPARE;	100ml Beaker, Syringe	MgSO4
28. SEPARATE;	Syringe;The DCM layer is the bottom layer.
29. DRY;		MgSO4
30. FILTRATE;	Erlenmeyer, Buchner
31. PREPARE;	250ml Beaker, Buchner, Erlenmeyer	50ml Acetone; Desired Acid
32. ADD;		Filtrated Organic Layer
33. ADD;		50ml Acetone
34. ADD;		Desired Acid
29. COOL;	Freezer
35. FILTRATE;	Erlenmeyer, Buchner
	220 Min.

 

[GDC]

I'm not sure about the timing... GAA -> Zinc -> NaOH ?? Max. Temperature ??

Step	Equipment	Chemicals
1. PREPARE;	Beaker 100ml	15g P2NP; 50ml Acetone
2. PREPARE;	Beaker 500ml	NaOH, H2O 1:1 Solution (200g;200ml)
3. PREPARE;	Beaker 150ml	NaOH, H2O 1:2 Solution (50g;100ml)
4. PREPARE;	Flask 250ml, Temperature Sensor, Reflux Condenser	50ml Acetone; 42g SnCl2; P2NP Solution;
5. ADD;		50ml Acetone; 42g SnCl2;
6. ADD;		P2NP Solution;
7. WORK; 20 Min.	Stirrer
8. PREPARE;	Beaker 150ml;	HCl Solution (150ml H2O; 4ml HCl
9. ADD; To Flask		HCl Solution
10. PREPARE;	Beaker 1000ml
11. ADD;		Transfer Mixture to Beaker
12. ADD;		400ml NaOH Prepared 1:1 Solution; !PH11!
13. PREPARE;	500ml Beaker, Buchner, Erlenmeyer, Syringe	Ethyl Acetate,MgSO4
14. EXTRACT;	Stirrer, Syringe	3x50ml Ethyl Acetate
15. DRY;		MgSO4
16. FILTRATE;	Erlenmeyer, Buchner
17. PREPARE;	500ml Flask, Stirrer	60ml GAA, 10g Zinc
18. ADD;		60ml GAA
19. ADD;		Mixtue of Oxime
20. ADD;		10g Zinc
21. WORK; 15 Min.	Stirrer
22. PREPARE	Buchner, Erlenmeyer
22. ADD;		150ml NaOH Prepared 1:2 Solution; !PH11!
23. FILTRATE;	Erlenmeyer, Buchner
24. PREPARE;	500ml Beaker, Buchner, Erlenmeyer	50ml DCM
25. ADD;	Filtrated Mixture
26. ADD;		50ml DCM
27. PREPARE;	100ml Beaker, Syringe	MgSO4
28. SEPARATE;	Syringe;The DCM layer is the bottom layer.
29. DRY;		MgSO4
30. FILTRATE;	Erlenmeyer, Buchner
31. PREPARE;	250ml Beaker, Buchner, Erlenmeyer	50ml Acetone; Desired Acid
32. ADD;		Filtrated Organic Layer
33. ADD;		50ml Acetone
34. ADD;		Desired Acid
29. COOL;	Freezer
35. FILTRATE;	Erlenmeyer, Buchner
	220 Min.

GDC

Add a cooled solution of sodium hydroxide (50 g in 100 ml water) to pH>10.

Are you add this as one portion or slow=How long? It reacts very exothermic

 

[TucoSalamanca.]

I got 5 grams of amphetamine from 15 grams of p2np.​

 

[GDC]

I got 5 grams of amphetamine from 15 grams of p2np.​

View attachment 37107

TucoSalamanca.How long do needed for the zinc part? (H2 Generation)

 

[TucoSalamanca.]

How to dry the product after filtration I do not have a vacuum filtration set

 

[GDC]

How to dry the product after filtration I do not have a vacuum filtration set

TucoSalamanca.Filtration with Coffee filter and acetone + let it dry on air.

 

[TucoSalamanca.]

Filtration with Coffee filter and acetone + let it dry on air.

GDCHow many ml of acetone should I add to my filter?

 

[GDC]

How many ml of acetone should I add to my filter?

TucoSalamanca.~5-10ml per g

 

[GDC]

How many ml of acetone should I add to my filter?

TucoSalamanca.and stir a little bit but with caution... another solution is a old jeans and press it

 

[GDC]

How to dry the product after filtration I do not have a vacuum filtration set

TucoSalamanca.How long did it take for the H2 generation with zinc? (Until the amin-base was ready)

 

[TucoSalamanca.]

How long did it take for the H2 generation with zinc? (Until the amin-base was ready)

GDCIt took 20 minutes

 

[GDC]

It took 20 minutes

TucoSalamanca.Did you cooled the Mixture?
Did you add all of the NaOH? Slow or Fast? (on both situations)
What was the maximum temperature while addition?

 

[TucoSalamanca.]

Did you cooled the Mixture?
Did you add all of the NaOH? Slow or Fast? (on both situations)
What was the maximum temperature while addition?

GDCI did not cool the mixture
In stage 2, yes, the reaction is indeed exothermic. I added it slowly.

 

[TucoSalamanca.]

Did you cooled the Mixture?
Did you add all of the NaOH? Slow or Fast? (on both situations)
What was the maximum temperature while addition?

GDCIf you want to make alkali, use sodium carbonate instead of sodium hydroxide. Maybe your problem will be solved. I use sodium carbonate.

 

[pingu]

View attachment 34800
Compared to the reduction of P2NP on aluminum amalgam, this method offers a significantly quieter reaction (The reaction isn't exothermic ), better yield (90%) and a very pure substance (no additional purification required).

Dissolve 15 g of P2N0 in 50 ml of anhydrous acetone

Spoiler: IMG 1

View attachment 34801

Place 100 ml round-bottomed flask on a magnetic stirrer equipped with a reflux condenser. Add acetone and 42 g of tin(II) chloride dihydrate

Spoiler: IMG 2

View attachment 34802

Turn on the stirring, wait for the tin chloride to dissolve and add the solution of P2NP in acetone

Spoiler: IMG 3

View attachment 34803

Stir for 20 minutes, the temperature rises slowly. A decrease in the temperature of the mixture indicates the end of the reaction. Place 150 ml of cold water and 4 ml 36% hydrochloric acid in a glass, slowly add to the mixture with stirring. The color of the solution changes

Spoiler: IMG 4

View attachment 34804

Prepare a solution of sodium hydroxide (200 g per 200 ml of water), cool it to room temperature and add to the mixture to pH>10 (in an acidic or neutral environment, extraction of oxime is impossible), a precipitate of inorganic salts immediately forms.

Spoiler: IMG 5

View attachment 34805

Extract 3 x 50 ml portions of ethyl acetate. dry with anhydrous magnesium sulfate. Place 60 ml glacial acetic acid in a beaker on a magnetic stirrer and add the solution that previously obtained (oxime in ethyl acetate).

Spoiler: IMG 6

View attachment 34806

While stirring, add 10 g of zinc dust.

Spoiler: IMG 7

View attachment 34808

Stir for 15 minutes.

Spoiler: IMG 8

View attachment 34809

Add a cooled solution of sodium hydroxide (50 g in 100 ml water) to pH>10.

Spoiler: IMG 9

View attachment 34810

Filter the mixture. add 50 ml dichloromethane, separate the organic layer, and additionally extract the aqueous layer 3 times with 20 ml DCM.

Spoiler: IMG 10

View attachment 34811

Organic extracts combined and dried over anhydrous magnesium sulfate.

Spoiler: IMG 11

View attachment 34814
View attachment 34815

We get a solution of 10 g amphetamine base in DCM. Add 50 ml of anhydrous acetone and the desired acid to obtain the corresponding salt.

Spoiler: IMG 12

View attachment 34816
View attachment 34817
View attachment 34818

yuiopjklCould you post a ingrediance list?

 

[GDC]

I think he is away

 

[GDC]

Could you post a ingrediance list?

pingu

1-Phenyl-2-Nitropropene	15​	g
Acetone	50​	ml
Sn(II)Cl * 2H2O	42​	g
Acetone	50​	ml
HCl	4​	ml
Water	150​	ml
NaOH	200​	g
Water	200​	ml
Ethyl Acetate	150​	ml
MgSO4	20% of the volume of final solution
ACETIC ACID (GAA)	60​	ml
Zinc	10​	g
NaOH	50​	g
H2O	100​	ml
DCM	110​	ml
MgSO4	20% of the volume of final solution
Acetone	50​	ml