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%
 

Pororo

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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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Dear, it looks you forgot that tartaric acid bonds two molecules of base. The same as sulphuric. You need to divide [ 0.01632 moles (2.45g/150.09g/mol) ] / 2 = 1.23
 

G.Patton

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75ckpt4HSC

1:1 same as for meth
 

Pororo

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Have you done this part by yourself?
I did. I was pretty surprised, with result, then I checked properties..
It works the same as sulphuric: one molecule of d or l tartaric acid bonds 2 molecules of base.
I guess there is the same mistake in your dextrometh explanation. Or excess of acid is added for some other technical reason, (reduce solubility for example)
 
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G.Patton

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How have you established this fact?
 

Pororo

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In certain solvents you see it clear, when your add acid salt starts to precipitate immediately.
You know the weight, so you know how much acid you need to add.
If you add a part of the whole acid, you may filter solids and add more, and see if salt precipitates or nor.
Salt stops precipitate approx as you reach molar 1:4.
Yield is around 95.
Try to do it, and you will see. Or better check tartaric acid spec.
 

Pororo

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http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/attachments/q6lca7lcd0-jpg.37905/
From this post.
 

G.Patton

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Hi. I read the source of this method again [attached to the post] and found that I was incorrect in my opinion but you also incorrect in yours, dear @Pororo.

As author said, two moles of phenylethylamine react with one mole of d-tartaric acid and form the solution of neutral salt d,l-phenylethylamine d-tartrate (as you said, 2 moles of amine and 1 mole of acid). D-phenylethylamine salt is dissolved in the solution while l-isomer is precipitated. So that my proportions are correct but meaning of my words in comments above was not.
BYkt8cau3g

I really appreciate for you notes and comments, you've helped to find mistake.
 

Pororo

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I don't know how you count, but of course there is NO ANY mistake in my calculations.
If you want to acidify the whole 1 mole of base with DL-tartaric, you need to use 0.5 mole of this acid.
If you want to extract only D or L from 1 mole of base with D or L-tartaric, you need to use 0.25 mole of D or L acid accordingly.
 

G.Patton

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I sent you above the quotation of Nabenhauer method. Please, read full article carefully. I tell the same.

In accordance with this article, if you take the proportion like you said (1moles amine with 0.25 moles of d-tartaric acid), you'll get 0.2-0.25 moles d-amine d-bitartrate in the precipitate from 1 moles of amine free base.

YPkdf9lQsb


The equasion of this reaction (from quotation):

1 mole d,l-amine + 1.2 mole d,l-tartaric acid = 0.5 mol of d-amine d-bitartrate (2 parts of amine bace per 1 part of acid)
the salt is precipitated

you take
1 mole d,l-amine + 0.25 mole d-tartaric acid = 0.25 mol of d-amine d-bitartrate as I suggest. Probably, you may get d-amine d-tartrate (1:1 base:acid) salt, which is also insoluble in this solvent. It's hard to predict. I haven't seen details of your experiment. Only your words.


If you wanna prove your argument, perform your experiment with pictures in comment section or new post.
 
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Pororo

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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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pocketknife

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@G.Patton Is this original write up or edited by u ?
This is nitroprop in IPA ? how do you keep p2np in solution from kristalising in the dripper ? ( kristals will block dripper).
Thank u
 

G.Patton

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Hello, It's carried out experiment in accordance with the method.
P.S. I don't understand your English. Please, reformulate your question.
 

pocketknife

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The solution in the addition funnel/ drip funnel is p2np in isoprop. alcohol?
When i try this ( p2np dissolved in hot isoprop. alcohol) my p2np starts to cristalizing in the glass addition funnel / drip funnel, because of temperature drop due to the (cold) glass funnel.
I hope u understand now ? ( sorry for the bad English)
 

G.Patton

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Yeah, Now it's much better =)
You can add more Isopropanol there but not too much.
 
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