XuTai10
Harmless
Posts: 5
Registered: 8-9-2011
Member Is Offline
Mood: No Mood
|
|
Synthesis of (d-ephedrine hcl)
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
Hazard to Others
Posts: 175
Registered: 20-5-2011
Member Is Offline
Mood: No Mood
|
|
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
International Hazard
Posts: 3975
Registered: 9-12-2002
Location: Estados Unidos de La Republica Mexicana
Member Is Offline
Mood: ....getting old and drowning in a sea of knowledge
|
|
........you've been given ample information at the vespiary, there isn' t. Any spoon feeding, if thats what you 're looking for......solo
It's better to die on your feet, than live on your knees....Emiliano Zapata.
|
|
|
Waffles SS
Fighter
Posts: 998
Registered: 7-12-2009
Member Is Offline
|
|
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
Hazard to Others
Posts: 109
Registered: 19-9-2008
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Others
Posts: 175
Registered: 20-5-2011
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Others
Posts: 109
Registered: 19-9-2008
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Self
Posts: 59
Registered: 13-7-2011
Member Is Offline
Mood: Barely any solvent in my emulsion
|
|
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)
This file has been downloaded 2137 times
|
|
|
Palladium
Harmless
Posts: 30
Registered: 17-1-2011
Member Is Offline
Mood: No Mood
|
|
| 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
Harmless
Posts: 14
Registered: 15-10-2011
Member Is Offline
Mood: No Mood
|
|
| 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
Harmless
Posts: 14
Registered: 15-10-2011
Member Is Offline
Mood: No Mood
|
|
| 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?
|
|
|
cipi
Harmless
Posts: 14
Registered: 15-10-2011
Member Is Offline
Mood: No Mood
|
|
Found if for you guys.
| 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
Harmless
Posts: 30
Registered: 17-1-2011
Member Is Offline
Mood: No Mood
|
|
| 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
Hazard to Self
Posts: 66
Registered: 9-7-2011
Location: USA
Member Is Offline
Mood: miserable fat slave
|
|
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
Hazard to Others
Posts: 109
Registered: 19-9-2008
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Others
Posts: 175
Registered: 20-5-2011
Member Is Offline
Mood: No Mood
|
|
| 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...
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
