Synthesis of Amphetamine from P2NP via SnCl2 and Zn

[TucoSalamanca.]

what can be used instead of magnesium sulphate

 

[mithyl2]

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]

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]

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]

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]

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]

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

 

[TucoSalamanca.]

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

 

[GDC]

~5-10ml per g

 

[GDC]

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

 

[GDC]

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

 

[TucoSalamanca.]

It took 20 minutes

 

[GDC]

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.]

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

 

[TucoSalamanca.]

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

 

[pingu]

Could you post a ingrediance list?

 

[GDC]

I think he is away

 

[GDC]

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