Author Topic: Simple Ephedrine.HCl Separation  (Read 505 times)

headstrong

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Simple Ephedrine.HCl Separation
« on: May 12, 2010, 10:29:07 AM »
Ephedrine.HCl solubility in water is about 25 g / 100 ml water at 25 c. And practically Ephedrine.HCl is insoluble in saturated NaCl-water solution.

Example 1;
I tried with 20 g HCl salt of Ephedra alkaloids, that is a mixture of Ephedrine.HCl, Pseudophedrine.HCl, PPA.HCL and methy Ephedrine.HCl.
1. Dissolve this crystal with 300 ml water, in 500 ml beaker glass, add NaCl by continuous stirring  till saturated, stirr well, smooth Ephedrine.HCl crystal will be precipitated out.
2. Filter, rinse with saturated NaCl-water solution.
3. Remove the NaCl by extract crystal #2 with anhydrous alcohol, filter the insoluble NaCl.

Example 2;
1.  Dissolve 20g  HCl salt of Ephedra alkaloid with 300 ml hot water (about 80 c), in 500 ml beaker glass, add NaCl by continuous stirring  till saturated. This time the temperature should be above 50 c, heat if necessary.
2. Let cool slowly, when the temperature reach about 25-30 c Ephedrine.HCl start to crystallize, big-long crystal like a grass, about 8cm length (depend on how slowly the temperature is dropped). Place in a fridge for 1 hour at ~10 c.
3. Filter, rinse with saturated NaCl-water solution.
4. Remove the NaCl by extract crystal #3 with anhydrous alcohol, filter the insoluble NaCl.

This way is also work for purification Ephedrine.HCl  from pills, and to separate it from any other substance that has a greater water solubility than NaCl. And if one do racemization to Ephedrine.HCl/Pseudophedrine.HCl, this procedure can be useful for separation.
And the good news this procedure is simple-easy as it said and high yielding.
Anyone willing to patent it? I give you for free ;D

iknowjt

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Re: Simple Ephedrine.HCl Separation
« Reply #1 on: May 14, 2010, 01:49:35 PM »

Anyone willing to patent it? I give you for free ;D

Headstrong I'm glad you yourself realize that you are an actual inventor.....mixed up among ramblers(myself included)
I look forward to more 'patent material' you have to share with this board

Anonymity

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Re: Simple Ephedrine.HCl Separation
« Reply #2 on: September 03, 2010, 12:17:40 AM »
Now I understand this post has since fallen to the realm of forgotten for the most part but I want to remind EVERYONE... This is the greatest thing that has ever come about for seperation of ephedrines from other substances including so called gakks. I want to kick myself for not thinking this sooner because its basic chemistry.

Take for instance an experiment performed trying to extract roughly 8 grams of ephedrine from TONS of other shit. They where extracted with EtOH repeatedly and evaporated recovering the left overs to remove the grams of TiO per 25mg of PSE and then washed in various solvents ect...ect....

Nothing was working very well and even when the crystals where formed they where coated in some sort of waxy substance that came along for the ride no matter what I threw at it.

It sat there for years in a milky solution that resisted all attempts to cleanse until lo and behold NaCl was added. Lots and Lots of it. Then it was heated and more NaCl was added until no more would go into a boiling solution.

This caused two things to happen in my case. First the "milkyness" was no longer soluble in the denser NaCl solution and was skimmed right off.

Second and best of all  on cooling the Ephedrine sulfate started to form great pin wheel shards growing bigger by the day. I could and would speed this up by condensing the solution further until NaCl started to precipitate while warm but no matter how you look at it the Ephedrine is always going to remove itself before the NaCl. After the fact wash with anhydrous Alcohol to remove any latent salt.


I asure every  pill washer to recrystalize your Ephedrine from a saturated NaCl solution. The gakks in no way shape or form stand a chance against this one and its simplicity and economic value is undeniable once its witnessed first hand. Be patiant and wait over night and you will be in awwww. Its been along time since I have seen crystals grow this large after the first precipitation. Normally it takes 2x recrystalization to get them this clean.

Sedit

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Re: Simple Ephedrine.HCl Separation
« Reply #3 on: September 04, 2010, 03:53:35 AM »
Not sure how I missed this head strong but I must say it is a beacon shining on the low level of knowledge that underground chemist of the day have.

I say this not because of your post but because of the lack of responce it has received. Any lesser soluble amine HCl salt beit Ephedrine, Amphetamines, MDA ectt... ect... friggin ect... will slowly precipitate as long as excess NaCl is added.

I understand your logic and slowly as the super saturated solution desires to solvate more NaCl it will be forced to slowly push more Organic HCl salt out of solution, an action that could take weeks at a time yet yeild three dee shaped crystals floating in solution. Its a work of art and I cant believe that folks took this long to think about it.


Now for my theory,

Hypothesis:

Disclaimer: As much as I dont want this forum in any, way, shape or form become a pill washing forum I feel this has a strong chemistry connection that applys to a massive amount of chemist and ALL should learn what headstrong is trying to teach here.



Theory stands as such for basic pills or organic plant matter.
Extract acidic solution of organic salt with boiling H2O,
add canning wax, the kind you get in blocks in the store,
Cool solution till wax hardens.
Filter anything that was not trapped in the wax like TiO( it could hold much of this as well mind you)
Take your clear aq solution and add alot of salt while hot until no more will dissolve.
Cool QUICKLY
Allow to stand for about 3 days to a week.
Filter.

You are left with NaCl (maybe )and organic HCL salt in large pure crystals I would assumre if I have ever tried this which I haven't.
grind in dry Alcohol that NaCl is not soluble in.
Filter and evaporate.....





Hmmmm just a theory but its chemistry based on the common ion theory..... LEARN IT!!!!!!




There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

hypnos

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Re: Simple Ephedrine.HCl Separation
« Reply #4 on: September 04, 2010, 06:54:34 AM »
very neat, I imagine this technique would this work for other water soluble compounds as well..what way would one use to ascertain the viability of this process with the compound they are working on--hey sedit could you elaborate a bit on the 'ion theory' please
"the two things you can give away and never lose, are what you know, and how you feel...."

poisoninthestain

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Re: Simple Ephedrine.HCl Separation
« Reply #5 on: September 05, 2010, 05:05:06 PM »
To impure pink/red MDA citrate mixed with excess citric acid monohydrate was added a minimal amount of dry IPA to get most of the solids to form a saturated solution. After addition IPA became dark cherry red and a mound of snow white crystals preciped to the bottom. IPA was decanted and crystals allowed to evap at room temp for several hours.  Melting point was not done but bioassay was positive with a much more bitter taste. If those same white crystals are added to dry IPA alone they go immediately into solution just as MDA citrate should. Muy facile.

It's good to hear similar stories with ephedrine.HCl ...nice! Good work headstrong! This has many applications with various amine salts...

poisoninthestain

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Re: Simple Ephedrine.HCl Separation
« Reply #6 on: September 08, 2010, 06:14:29 PM »
very neat, I imagine this technique would this work for other water soluble compounds as well..what way would one use to ascertain the viability of this process with the compound they are working on--hey sedit could you elaborate a bit on the 'ion theory' please

common ion effect is when two ionic substances sharing one or more ions in common supresses the solubility of another based on the conjugate acid or base strength precipitating the weaker one...in this example NaCl and hydrochloride salts of amines both share common anions and due to the difference between them salts out the amine hydrochloride...same if one is using citrates/citric acid system or another pair.

hypnos

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Re: Simple Ephedrine.HCl Separation
« Reply #7 on: September 12, 2010, 10:52:02 AM »
thanx poisonstainman exactly the succinct and savvy type of answer i was lookin for 8)......no doubt sedit could havedone the same, but youu beat him to it!!! ;D
"the two things you can give away and never lose, are what you know, and how you feel...."

Sedit

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Re: Simple Ephedrine.HCl Separation
« Reply #8 on: September 12, 2010, 05:17:47 PM »
As much as I am busy anymore you can pretty much bet everyone will beat me to everything for a while. I felt better allowing someone else to explain it because there are many here much more qualified then myself to do so. I am hoping for someone to teach me a little something on the order of how much of the precipitating anion will remain in solution in accordence to acid/base theorys. As to say will another chloride provide better precipitation of a hydrochloride amine salt and they numbers behind this increased precipitation or equilibrium constants.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

WizzBang

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Re: Simple Ephedrine.HCl Separation
« Reply #9 on: September 15, 2010, 09:59:20 PM »
Sedit for what it's worth the Wizz took notice and huge interest in this thread almost as soon as it was posted, by dumb luck actually. Haven't gotten too much into it due to SwiM's inexperience, and especially here will make sure one's i's are dotted and t's crossed before posting his thoughts and results with it. Thanks to headstrong, this might bee something wonderful :D

poisoninthestain

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Re: Simple Ephedrine.HCl Separation
« Reply #10 on: September 16, 2010, 03:29:59 AM »
APAP/pseudo.HCl NaCl extractions have not worked for myself.  However the others have.

atara

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Re: Simple Ephedrine.HCl Separation
« Reply #11 on: September 16, 2010, 05:45:36 AM »
Uhm. How much phenylpropanolamine is there? You may be throwing out the baby and keeping the bathwater if you're throw out PPA and keep ephedrine, but if the PPA yield is tiny, then fuck it.

headstrong

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Re: Simple Ephedrine.HCl Separation
« Reply #12 on: October 12, 2010, 12:00:56 AM »
Thanks for the feed back :)
Quote
As much as I don't want this forum in any, way, shape or form become a pill washing forum

I like pills extraction, but i don't like when people only looking for easiest way to obtain the  final product without enjoying the process.  Entire board will be diluted by skin deep questions about washing, easy way, etc, i don't like it at all. For me, no worries i can gladly keep my self avoid posting anything specific about pills.

For Ephedrine.HCl in this procedure, only takes hours or over night max, Ephedrine.HCl will be crystallized (almost) completely, dunno for other may be take take time longer to weeks.


Quote

To impure pink/red MDA citrate mixed with excess citric acid monohydrate was added a minimal

amount of dry IPA to get most of the solids to form a saturated solution.
Thanks for this info.


Quote
a little something on the order of how much of the precipitating anion will remain in solution

in accordence to acid/base theorys. As to say will another chloride provide better precipitation

of a hydrochloride amine salt and they numbers behind this increased precipitation or

equilibrium constants.

I'm not good in theory, but as i remember from 15 g alkaloid (after A/B and tone wash) i get 13 g Ephedrine.HCl (containing a little NaCl), and still got above 90% when i repeated the process to those crystal.

Pseudoephedrine.HCl and other that has a greater solubility than NaCl left as solute, it was proven when i did A/B to extract them, then i performed the procedure (with les volume of water), no precipitation was occured.
Doesn't work for Methamphetamine.HCl too, not in hours neither over night.


Quote

common ion effect is when two ionic substances sharing one or more ions in common supresses the

solubility of another based on the conjugate acid or base strength precipitating the weaker

one..

No, this related to the solubility of each salt and not related to ion strength. Similar like when Ca(OH)2 is added into Na2(CO3) solution, then we will get NaOH solution and precipitation of Ca(CO3) among with Ca(OH)2, and finally Na2(CO3) will be precipitated after that solution saturated with NaOH.


Quote
APAP/pseudo.HCl NaCl extractions have not worked for myself.  However the others have.

Your experiment was right, dunno how but they were wrong.
Years ago i ever crystallized 15 g PSE.HCl in 800 ml 37% HCl then added ZnCl2 to (almost) saturated. 37% HCl is useless, can be replaced by water, or  even better if the solvent is IPrOH (to reduce the amount of ZnCl2).
But what the purpose to do it to PSE? I dont see any value in mahuang alkaloid separation or even in pills extraction.

If any part of my post is rough or impolite, please forgive me i really don't mean to, my English is bad and i'm not a good writer.