Dextroamphetamine Synthesis (Nabenhauer, 1942)

G.Patton

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We took 6g of racemate = 3 g of D-amph+3 g of L-amph
We got
2.63g yield = x%
3.0g theory = 100%

2.63*100/3=87.7%
 

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Thanks for an interesting study. But I'm surprised with your tartaric acid proportions.
6g of amph sulphate is 3.49 g of racemic amph base. Then why do you use 2.45 g of d-tartaric? It shall come in molar proportions 1:4, i.e. 0.97g of d-tartaric is enough???
 
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Pororo

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sorry, I also made a mistake in calculations.
6g of amph sulphate is 4.41 g of racemic amph base. D-tartaric in molar proportions 1:4 is 1.23g as it is the same as suplhate: 1 mole of acid per 2 moles of amph. 2 times less than you count it.
 

G.Patton

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Hello, 6g of amph sulphate (368.5 g/mol) contain 0.03256 moles free base (look at the reaction equasion, where 2molecules of amph produce 1molecule of salt and vice versa). Briefly, one mole of sulphate salt contain two moles of free base, hence moles of amph sulphate multiply x2 (0.01628x2).

Your question is why it's written to take 2.45g of d-tartaric acid.
Answer: 2.45g of d-tartataric acid is 0.01632 moles (2.45g/150.09g/mol). Hence, this 0.01632 moles (2.45g) is half of 0.03256 moles of racemic amph free base.
You need 1/2 cuz this racemic amph free base contains 1/2 of d-amph and l-amph in theory.

Do you understand?
 

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I got your idea. I don't know why you believe you are going to get bitartrate. May be because of ethanol.

If I understand terms correctly, tartrate means 1:2, but bitartrate means 1:1 molar proportions!!!

But I don't use ethanol. I use other solvents.

What I know, crystallization stops as soon as 0.25 moles of acid consumed with yield 95%. Then, if 0.25 moles of opposite acid is added, precipitation will start again with yield 95%.
And now, when 0.25 of L and 0.25 of D were applied, if I try to add more D or L or DL acid to mother liquor - nothing happens. It looks there is no base, ph is also acidic.
For the prove, may be, may be, on occasion. Not sure when I will do amph separation again, end of September may be.
 
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Pororo

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I think, the point is here mr. Patton, and it is very simple: sequence fucking matters!!!

1. If you have a flask with with 1 mole of tartaric acid, d or l or dl, whatever, and start adding 1 mole of corresponding base in small portions, in the result you will get mostly bitartrate and some tartrate (+ some unreacted acid probably) with salt's resulting PH = 2.
2. This is what I do! If you have a flask with with 1 mole of base and start adding 0.5 mole of tartaric acid in small portions, in the result you will get mostly tartrate and some bitartrate (+ some unreacted acid.) with salt's resulting PH = 5.0-5.5.
Or 1 mole of racemic base and 0.25 mole of d or l acid if you are targeting to separate them
 
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JoshL1221

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hi, excuse me, when you say "We precipitate d-amphetamine with an additional amount of d-tartaric acid.", how much d-tartaric acid is used? thanks.
 

G.Patton

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Same as in the previous addition with a little excess.
 

Ihml

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Could d-aspartic acid be used instead of d-tartaric acid?
 

Ihml

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Would the lack of solubility of d-aspartic acid in isopropyl alcohol be a problem?
 

handle

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Can D,L Tartaric Acid can be used?
 

handle

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of course not, that would be to easy.. (L)Tartaric acid is extremely expensive here..(D) does not exist here.
Could we use Camphorsulfonic acid instead?
 

Ihml

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L-tartaric acid is like 10 euros per 1 kg where I live. Where are you from?
 

handle

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M3erHqoMFB

Plus some ridiculous freight charge on top.
 

G.Patton

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Order that from China here, it would be much cheaper.
 

handle

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Would Camphorsulfonic acid work?
Otherwise I will buy Tartaric Acid from China.
 

G.Patton

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I don't know for sure. Probably. There are questions about its solubility and amphetamine adduct solubility with this acid.
 

handle

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When doing the initial salting of the freebase, no precipitation forms? The freebase is now slightly acidic with no product. Can I save it from here? Or is it now rubbish?
 

G.Patton

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Hi, can you be more precise with your question please.
 

FENTAMAS

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@handle, International team of telepathic chem experts already working with your problem.
Wait for a Skype call when the solution is ready.

But some info is already accessible from universe, we guess the reason is WATER.
 

handle

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Eye eye captain., I'll try it again, this time on a boat? Water, water everywhere but not a drop to drink.
 

dummy dummietis

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What solvents in what proportions shall be used to extract d-amph from racemic?
Of course, I can separate isomers in acetone, but it requires a lot of acetone, around 15+ml per 1g of racemic base. I'm looking for more fast route. Better if salt and unreacted base will stay in different phases after partial acidation.
 
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