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Topic: Synthesis of (d-ephedrine hcl)  (Read 10288 times)

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Offline XuTai10

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Synthesis of (d-ephedrine hcl)
« on: December 18, 2011, 03:00:07 PM »
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)

Offline Arkcon

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Re: Synthesis of (d-ephedrine hcl)
« Reply #1 on: December 18, 2011, 03:21:46 PM »
Your synthesis method appears to be typical from what I've gleaned online.  I don't really see what the source of confusion is for you -- the yield may be low, but that is typical for this synthesis. 

http://en.wikipedia.org/wiki/Ephedrine#Synthesis

The molecule in question is a controlled substance, so clear and easy procedures for mass production isn't something people usually talk about on open forums.  Maybe someone at a local university or manufacturer would like to work closely with you?
Hey, I'm not judging.  I just like to shoot straight.  I'm a man of science.

Offline XuTai10

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Re: Synthesis of (d-ephedrine hcl)
« Reply #2 on: December 18, 2011, 03:59:24 PM »
I think that the hydrogenation is not bad except for some deficiencies as a small amount of catalyst. However, I have a problem with the insulation product after hydrogenation, which is the major product (l-ephedrine), and it can not insulate as best practices. The method for the isolation of (l-ephedrine) I have found in practice to try. I need advice on the synthesis of d-ephedrine hcl.
Or recommend me some literature or practical skills of processing.

Offline Hurat

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Re: Synthesis of (d-ephedrine hcl)
« Reply #3 on: December 18, 2011, 04:12:57 PM »
Typical junkie trying to make Methamphetamine.

Please lock this thread.

Offline XuTai10

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Re: Synthesis of (d-ephedrine hcl)
« Reply #4 on: December 18, 2011, 04:24:14 PM »
That you're wrong, I'm no junkie.

Offline discodermolide

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Re: Synthesis of (d-ephedrine hcl)
« Reply #5 on: December 18, 2011, 04:29:02 PM »
Sorry to say this but your English is so bad in the original post that I do not understand what information you are after.
Please do not attempt to make controlled substances unless you are employed inn the pharma sector. Even then it is difficult as you must account for every mg of starting material and product you prepare.
Development Chemists do it on Scale, Research Chemists just do it!
My Research History

Offline XuTai10

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Re: Synthesis of (d-ephedrine hcl)
« Reply #6 on: December 18, 2011, 04:55:20 PM »
I will explain it a bit. I got the award for finding a solution to this problem. I work in the theoretical part of the research as a project manager. I'm not privy to the field. However, I'm trying to find a material that could be applied to this process. Any comments like "it's like a drug addict and" are not in place.

Just ask for help in solving your problem or suggestions how this process should look like. It is not yet an industrial production.

Offline Arkcon

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Re: Synthesis of (d-ephedrine hcl)
« Reply #7 on: December 18, 2011, 05:33:35 PM »
We're sorry XuTai10: we don't mean to say that you're a junkie.  But any information we type here and leave for everyone to see can be used by junkies, and we would be blamed.  That is what I mean when I said, this is a controlled substance, and we can't give you too much specific help.  From what I understand from your second post, you're having trouble purifying the correct enatiomer.  I'm not surprised, Wikipedia says that the product is crystallized, and the resulting crystals are sorted.  Yikes.  Worked for Louis Pasteur, but not the way I'd like to spend my day.  If I worked for a major pharmaceutical company, and I had a shortcut, I wouldn't release it to the public, it would both be too valuable and to dangerous.  I think its time to lock this thread.  I hope you'll stick around for more theoretical questions.

http://en.wikipedia.org/wiki/Louis_Pasteur#Work_on_chirality_and_the_polarization_of_light
Hey, I'm not judging.  I just like to shoot straight.  I'm a man of science.

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