Sciencemadness Discussion Board

Synthesis of (d-ephedrine hcl)

XuTai10 - 18-12-2011 at 01:11

Hi all.
I'm trying to develop a method of production (d-ephedrine hcl) by active amination and hydrogenation on palladium catalyst under U.S. Patent No. 7,176,332 B2, where there is a main product (l-ephedrine). During this hydrogenation to meet with several uncertainties. The resulting mixture of hydrogen, even if the reactants are not in the liquid crystalline state but it is. It is not possible, these crystals dissolve in ether but only in the water.

After dissolution of the crystalline mixture of hydrogen sever unreacted L-PAC and the rest of the mixture do synthesis using acetic acid and acetan chloride. Then mix in a vacuum, and sever the remainder of the mixture crystallizes with acetone. This creates scaly crystals with melting point 220 ° C for pure clean.

Of the total 200 g of hydrogenated L-PAC yield 45 g I in crystalline form (l-ephedrine).

Would anyone be willing to help me with this problem? Request (d-ephedrine hcl)

[Edited on 18-12-2011 by XuTai10]

simba - 19-12-2011 at 15:59

Why did you choose hydrogenation anyway? There are easier routes out there.

Hydrogenation is better for large scale production only. Or is that your case?

[Edited on 20-12-2011 by shivas]

[Edited on 20-12-2011 by shivas]

[Edited on 20-12-2011 by shivas]

solo - 19-12-2011 at 17:29

........you've been given ample information at the vespiary, there isn' t. Any spoon feeding, if thats what you 're looking for......solo

Waffles SS - 19-12-2011 at 23:30

Why you want to make d-ephedrine?you want to make meth?if yes then i think there is better way for make that
What about P2P amination then hydrogenation(after that maybe resolution.up to you)?huh?by this method you can make large amount of meth and sell that to get rich.
Like breaking bad tv serial and sure this is not important that :
How many people will die (not important!)
How many people get trouble(not important!)
How many people get sick(not important!)
How many people Loss their family(not important!)
Let me say what is important:Fucking Money. isnt it?



[Edited on 20-12-2011 by Waffles SS]

pip - 21-12-2011 at 10:44

l-pac gives l-ephedrine which gives d-meth he wants d ephedrine which gives l-meth or whats in vicks inhalers. He either wants to sell medical meth for the vicks inhalers or is a total retard and thinks d-ephedrine = d-meth. In cases like this its great the d-l thing is confusing as hell to noobs and never consistant when your modifing molecules.

besides how does he plan on getting dpac from nature? or am I the idiot and the optical polarization changes in the pac to ephedrine stage not the ephedrine to meth stage?




[Edited on 21-12-2011 by pip]

simba - 21-12-2011 at 11:40

Quote: Originally posted by pip  
l-pac gives l-ephedrine which gives d-meth he wants d ephedrine which gives l-meth or whats in vicks inhalers. He either wants to sell medical meth for the vicks inhalers or is a total retard and thinks d-ephedrine = d-meth. In cases like this its great the d-l thing is confusing as hell to noobs and never consistant when your modifing molecules.

besides how does he plan on getting dpac from nature? or am I the idiot and the optical polarization changes in the pac to ephedrine stage not the ephedrine to meth stage?
[Edited on 21-12-2011 by pip]


L-PAC is made my condensation of benzaldehyde with pyruvate catalyzed by pyruvate decarboxylase. R-PAC(the one which gives d-ephedrine) can be made by the same process by using acetolactate synthase enzyme.

[Edited on 21-12-2011 by shivas]

pip - 21-12-2011 at 11:45

ok, I never looked into meth syntheses too much just from what I read levo is natural the other is unnatural except for rare occasions.

Alastair - 21-12-2011 at 13:36

If you are trying to get only one isomer there probably will be some very low yield involved.
Pricy palladium salts/catalysts would be wasted inefficiently. I think industry uses benzaldehyde>phenyl 1propanol 2 ketone and reductive amination later and somehow gets just one (levo) isomer.


Attachment: US1956950.pdf (105kB)
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Palladium - 26-12-2011 at 12:33

Quote: Originally posted by XuTai10  
Hi all.
I'm trying to develop a method of production (d-ephedrine hcl) by active amination and hydrogenation on palladium catalyst under U.S. Patent No. 7,176,332 B2, where there is a main product (l-ephedrine). During this hydrogenation to meet with several uncertainties. The resulting mixture of hydrogen, even if the reactants are not in the liquid crystalline state but it is. It is not possible, these crystals dissolve in ether but only in the water.

After dissolution of the crystalline mixture of hydrogen sever unreacted L-PAC and the rest of the mixture do synthesis using acetic acid and acetan chloride. Then mix in a vacuum, and sever the remainder of the mixture crystallizes with acetone. This creates scaly crystals with melting point 220 ° C for pure clean.

Of the total 200 g of hydrogenated L-PAC yield 45 g I in crystalline form (l-ephedrine).

Would anyone be willing to help me with this problem? Request (d-ephedrine hcl)

[Edited on 18-12-2011 by XuTai10]


I couldn't find Palladium in this US Patent, but for me it sounds very strange to use Palladium for reductive amination or alkylation. Simply because that's not the preferred catalyst, and I doubt it work more than helpful.

Platinum can reduce amination of both ephedrine and norephedrine, but the latter in not so good yields.

Amalgated aluminium is here mentioned, and do so if you like to spend much time for less. It works, but takes much solvent and time. It's an expensive way of making Ephedrine. The time of prepare this poison to catalyst, and relatively big amount of the materials to it, for a relatively small batch. The smell of fizzling hydrogen in your solvent will occupy your entire house, and it's also a significant risk for fire. I can make the list even longer about the backdrafts of using this catalytic hydrogenation method. Take care of your health when reducing, and make sure you know how to get rid of all the mercury when reduction is finished.

[Edited on 26-12-2011 by Palladium]

[Edited on 26-12-2011 by Palladium]

cipi - 28-12-2011 at 10:35

Quote: Originally posted by pip  
l-pac gives l-ephedrine which gives d-meth he wants d ephedrine which gives l-meth or whats in vicks inhalers. He either wants to sell medical meth for the vicks inhalers or is a total retard and thinks d-ephedrine = d-meth. In cases like this its great the d-l thing is confusing as hell to noobs and never consistant when your modifing molecules.

besides how does he plan on getting dpac from nature? or am I the idiot and the optical polarization changes in the pac to ephedrine stage not the ephedrine to meth stage?




[Edited on 21-12-2011 by pip]


Isn't there a way to get norephedrine by using a different solvent during the hydronation of lpac? (I remember ethanol being used andin the pressure required is only 15 psi...) I remember reading this here at sciencemadness -so?- I don't remember which isomer is formed which is important. Ill find it for you guys...

cipi - 28-12-2011 at 10:41

Quote: Originally posted by shivas  
Quote: Originally posted by pip  
l-pac gives l-ephedrine which gives d-meth he wants d ephedrine which gives l-meth or whats in vicks inhalers. He either wants to sell medical meth for the vicks inhalers or is a total retard and thinks d-ephedrine = d-meth. In cases like this its great the d-l thing is confusing as hell to noobs and never consistant when your modifing molecules.

besides how does he plan on getting dpac from nature? or am I the idiot and the optical polarization changes in the pac to ephedrine stage not the ephedrine to meth stage?
[Edited on 21-12-2011 by pip]


L-PAC is made my condensation of benzaldehyde with pyruvate catalyzed by pyruvate decarboxylase. R-PAC(the one which gives d-ephedrine) can be made by the same process by using acetolactate synthase enzyme.

[Edited on 21-12-2011 by shivas]


Can you please give us the reference that supports this?

Found if for you guys.

cipi - 28-12-2011 at 11:35

Quote: Originally posted by Organikum  
Quote:

orgy, i aim for ppa from l-pac..


Norephedrine form l-PAC:
Pressurerized Al/Hg as on Rhodiums page but with ammomia in ethanol (94% alc. is ok). Yield: 50% to 60%.
Add the amine in alcohol to the ketone and let sit for some hours. This should warm up on addition. Then do the Al/Hg under pressure (3 to 5 atm is ok).
Ratios amine to ketone 1 to 1,5 molar.

your milage may vary
/ORG

Palladium - 28-12-2011 at 14:49

Quote: Originally posted by cipi  
Quote: Originally posted by Organikum  
Quote:

orgy, i aim for ppa from l-pac..


Norephedrine form l-PAC:
Pressurerized Al/Hg as on Rhodiums page but with ammomia in ethanol (94% alc. is ok). Yield: 50% to 60%.
Add the amine in alcohol to the ketone and let sit for some hours. This should warm up on addition. Then do the Al/Hg under pressure (3 to 5 atm is ok).
Ratios amine to ketone 1 to 1,5 molar.

your milage may vary
/ORG


This is a relatively low-yielding route. The reason is because this isn't the preferred catalyst. With NH3 in EtOH this is supposed to be with Raney Nickel with high H2 pressure.

The primary amine of PEA I haven't seen any result over ~50% with any other catalyst than RaNi.

overload - 28-12-2011 at 20:38

I believe that Palladium. The idea of brewing lpac was flattering a few years ago but I never pursued. I've still been interested in yeast and the chemical reactions they can carry out for us. The patent I read through today was veery cool. It explained how the yeast are mutated and placed in an atmosphere of acetaldehyde fumes. The mutated ones that gain the ability to survive high levels of acetaldehyde live and the others die. The survivors are cultured and used for producing higher yields. No point in actually going through with it since I have no use for ephedrine. All you can get from ephedrine is a severely bashed dopamine and serotonin system if, for example, you decided to produce large quantities of methcathinone and methamphetamine.

pip - 9-1-2012 at 00:55

I dont give a crap about meth but why when making lpac isn't dpac made if it can be with the other enzyme? Is it the obvious, yeast doesnt have that enzyme?I

[Edited on 9-1-2012 by pip]

simba - 22-5-2012 at 18:26

Quote: Originally posted by cipi  
Quote: Originally posted by shivas  
Quote: Originally posted by pip  
l-pac gives l-ephedrine which gives d-meth he wants d ephedrine which gives l-meth or whats in vicks inhalers. He either wants to sell medical meth for the vicks inhalers or is a total retard and thinks d-ephedrine = d-meth. In cases like this its great the d-l thing is confusing as hell to noobs and never consistant when your modifing molecules.

besides how does he plan on getting dpac from nature? or am I the idiot and the optical polarization changes in the pac to ephedrine stage not the ephedrine to meth stage?
[Edited on 21-12-2011 by pip]


L-PAC is made my condensation of benzaldehyde with pyruvate catalyzed by pyruvate decarboxylase. R-PAC(the one which gives d-ephedrine) can be made by the same process by using acetolactate synthase enzyme.

[Edited on 21-12-2011 by shivas]


Can you please give us the reference that supports this?


http://onlinelibrary.wiley.com/doi/10.1002/bit.10728/abstrac...