Dextroamphetamine synthesis (Nabenhower, 1942)

[Amphibian]

I've tried to look but can't really find an answer for pd/c preparation
I have activated carbon and maybe 50g of palladium chloride made by dissolving palladium in aqua rega and bubbling chlorine through which dropped out a nice dark red salt looks a little like iron oxide. And dried to constant weight.
How do I make pd/c
Sorry a bit off topic.
Is pd/c pyrophoric?

Evilcarrot2Palladium Catalyst Preparation (haven't tried it out)

 

[Evilcarrot2]

Wow than

Palladium Catalyst Preparation (haven't tried it out)

AmphibianWow thanks exactly what I've been looking for

 

[G.Patton]

Is pd/c pyrophoric?

Evilcarrot2I don't think so.

How do I make pd/c

Wikipedia said:
A solution of palladium chloride and hydrochloric acid is combined with aqueous suspension of activated carbon. The palladium(II) is then reduced by the addition of formaldehyde. Palladium loading is typically between 5% and 10%. Often the catalyst mixture is stored moist.

I've never prepared Pd/C by myself.

 

[diogenes]

can somebody explain me again pls what would be the difference if I use l-tartaric instead of d-tartaric acid with freebase? with l-tartaric there would precipate what? the d-amphetamine l-tartaric salt? What would I do then?

finch3523When you switch the tartaric acid isomers, then everything is simply the other way round. The amph isomer which was in the organic phase will be in the water and the salt (water soluble) will be in the organic. I know some people use the L tartaric acid (despite more difficult to get) because then the D amphetamine will be in the water phase.

 

[PhantomFeatherSword]

Excuse the amateur question, but when I was reading about tartaric acid on Wikipedia, there was a line that confused me a bit:

Naturally occurring form of the acid is dextro tartaric acid or L-(+)-tartaric acid (obsolete name d-tartaric acid). Because it is available naturally, it is cheaper than its enantiomer and the meso isomer. The dextro and levo prefixes are archaic terms.

When I read the above "dextro tartaric acid or L-(+)-tartaric acid", I kinda read it as "dextro tartaric acid AKA L-(+)-tartaric acid".
Which makes me wonder, if I'm trying to isolate the dextroamphetamine isomer, should I be buying the L-(+)-tartaric acid (like this)? Or the D-(-)-Tartaric Acid (like this)? Im really hoping it's the D-(-)-Tartaric Acid, because that's what I already have.

 

[G.Patton]

Excuse the amateur question, but when I was reading about tartaric acid on Wikipedia, there was a line that confused me a bit:

When I read the above "dextro tartaric acid or L-(+)-tartaric acid", I kinda read it as "dextro tartaric acid AKA L-(+)-tartaric acid".
Which makes me wonder, if I'm trying to isolate the dextroamphetamine isomer, should I be buying the L-(+)-tartaric acid (like this)? Or the D-(-)-Tartaric Acid (like this)? Im really hoping it's the D-(-)-Tartaric Acid, because that's what I already have.

PhantomFeatherSwordHello, you can use both of them. I wrote the method for L-tartaric acid. Read comments above. Your question is already discussed several times.
Also, read this theme.

 

[Midget_Impinger]

Extraction of d-amphetamine​

We've got racemic amphetamine. It contains 1 molecule of d-amphetamine per 1 molecule of l-amphetamine. Next, 6 g of racemate is taken and dissolved in 6 ml of water, an alkali solution is added to reach pH = 11.​

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Extract with 5 ml of petroleum ether and warm the solution, add 2.45 g of d-tartaric acid in alcohol solution to the mixture. Then add alcohol until completely dissolved and cool with stirring. The l-amphetamine d-tartaric salt precipitates. The d-amphetamine remains in the solution. You can repeat procedure of cleaning precipitate of l-amphetamine d-tartaric salt by methanol to increase yield.​

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We precipitate d-amphetamine with an additional amount of d-tartaric acid. We filter the precipitate, get the base of d-amphetamine, adding alkali to pH = 11.

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We acidify the d-amphetamine base to pH = 6 with a solution of sulfuric acid in acetone. This gives 2.63 g of d-amphetamine sulfate. Yield is 2.63 / 3 = 87.7%

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This extraction method valid to amphetamine, which was synthesized by any routes. There is another way to obtain dextroamphetamine.

G.Patton@G.Patton - Is this optical resolution process using d-tartaric acid applicable to other amphetamines? Specifically 4-fluoroamphetamine, 4-fluoromethamphetamine and plain ol methamphetamine?

 

[G.Patton]

@G.Patton - Is this optical resolution process using d-tartaric acid applicable to other amphetamines? Specifically 4-fluoroamphetamine, 4-fluoromethamphetamine and plain ol methamphetamine?

Midget_ImpingerHello, yes, it is.

 

[Ra226]

How to separate the chiral isomers of methamphetamine?Can this amphetamine technique be applied to methamphetamine?

 

[UWe9o12jkied91d]

How to separate the chiral isomers of methamphetamine?Can this amphetamine technique be applied to methamphetamine?

Ra226Yes, it is the same

 

[41Dxflatline]

I've always added GAA and sometimes used 80% acetic acid too but later today I'm going to try without acetic acid at all. What ratio of IPA:Water do you use in your P2NP solution?

 

[G.Patton]

I've always added GAA and sometimes used 80% acetic acid too but later today I'm going to try without acetic acid at all. What ratio of IPA:Water do you use in your P2NP solution?

41DxflatlineHello

Pour 30 ml of water into the flask, insert a thermometer into the left throat of the flask, insert a reflux condenser into the central throat, and insert a dropping funnel with 110 ml of 14% P2NP (it is phenylnitropropene; 1-phenyl-2-methyl-2-nitroethylene) solution into the right throat.

 

[UWe9o12jkied91d]

I've always added GAA and sometimes used 80% acetic acid too but later today I'm going to try without acetic acid at all. What ratio of IPA:Water do you use in your P2NP solution?

41DxflatlineI've heard people use half of GAA, i used full GAA equivalent and still went fine, both ways are fine

 

[41Dxflatline]

I've heard people use half of GAA, i used full GAA equivalent and still went fine, both ways are fine

UWe9o12jkied91d
Seems to be going ok:

https://imgur.com/a/37WuR3e

 

[nsrnsr]

Extract with 5 ml of petroleum ether and warm the solution...
May I ask what does it mean to extract?

 

[G.Patton]

Extract with 5 ml of petroleum ether and warm the solution...
May I ask what does it mean to extract?

nsrnsrExtraction one substance from a solution with help of an appropriate solvent.
Extraction

 

[nsrnsr]

Extraction one substance from a solution with help of an appropriate solvent.
Extraction

G.PattonIs it okay to use ether? Thank you

 

[G.Patton]

Is it okay to use ether? Thank you

nsrnsrDo you mean diethyl ether (Et2O)? Yes, of course.

 

[nsrnsr]

May I ask whether to add d-tartaric acid first or extract first? Thank you

 

[G.Patton]

May I ask whether to add d-tartaric acid first or extract first? Thank you

nsrnsrOf course you need extract amph free base before. In opposite case the acid will reacts with alkali (NaOH or KOH).