extracting pfed hcl with h2o/ipa as a pre

[Vaaguh]

In a 200 ml beaker there where 200 72mg PseudoEphedrine HCl pills dissolved in 100 ml h2o/50 ml IPA and brought up to boiling under magnetic stirring.

After 15 minutes 50 ml conc hcl was added and the pills where dissolved.

10 minutes later the slurry white mass was gravity filtered and a slightly offwhite yellowish colored liquid remained.


My question is, as PseudoEphedrine HCl is very soluble in water is there any possibilty (perhaps known additives the box didnt say anything about the non medical ingredients) that some PseudoEphedrine HCl did not dissolve into the warm H2O/Ipa mixture?

If the PseudoEphedrine Hcl is in the solution then would following the "Straight to E" procedure after evaporation of the h2o/IPA give good results?

[SHORTY]

I would say the psuedo is most definetly in the solution.

A few questions:

1.  Why did you do it this way?

2.  Did it take along time to filter?

3.  What happened after you added the hcl?

4.  Was there alot of solids in the filter?

Im not being a smartass i really am interested.  You may have found a simpler and easier way to extract pseudo.  Although there surely is some gaak still in the solution it might be a good start.

Evap the solution on low heat and crash with acetone then weigh and proceed with the ste.

Look forward to hearing the results.

[Vaaguh]

1.  Why did you do it this way?
Trying to get the PseudoEphedrine Hcl into the solution as efficient as possible, as off the hcl it was an attempt to break up anything that was crystalline.

2. Did it take along time to filter?
No it filtered easy and fast and a serious ammount powder was filtered out tomorrow the weight of how much residual powder/crap retreived shall be checked.

3.  What happened after you added the hcl?
The solution cleared up a little at first and after a while there where no more chunks in he solution

4.  Was there alot of solids in the filter?
Yes.

There was no time today to slowly evap most of the H2O/Ipa but as soon as things are evaporated the residual crystals will be washed with acetone first and optionally with MEK and from there perform a meltpoint test.

[SHORTY]

Im gonna have to get some pills and do some experimenting!  I think you might be on to something here.  Any idea on what the inactives were in the pills?  Was there any antihistamine like tripolidine in them?  Have you tried this without the h2o?

[geezmeister]

The 72 mg tablets of pseudo I have found can be pulled with IPA or MeOH alone. You mention that you do not know what the inactive ingredients of the pills are.  If the pills are the 72 mg ones I have used, the Straight to E would work very well with no other cleaning or preparation of the pills.

Adding some HCl to the solution to break some of the gaks in the pills has been the subject of earlier posts, which (to the best of my recollection) were largely inconclusive as to benefits obtained, if any. If you boiled these pills for fifteen minutes in a water/alcohol soultion, they should have already been dissolved before you added the HCl. I doubt the HCl is needed here. Many of the OTC pseudo pills contain water-activated extraction blockers. The last time I extracted from the 72 mg pills they did not have any. Extracting pseudo with water from OTC pills when you do not know the inactives present is a open invitation to a big gooey mess and low yields.

The pseudo from the pills should all be in the H2O/IPA/Hcl solution.  when you finish evaporating it, rinse well with acetone to remove the excess HCl. Unless the pseudo is obviously contaminated, recrystalizing it a couple of times should be sufficient to get it clean. You could also  precipitate the pseudo from an alcohol solution in xylene by boiling off the alcohol. That is simpler than the full straight to E process, and for cleaning extracted pseudo of its final contaminants just as effective. I have done it after less-than-pristine extractions using the straight to E with good success.

Post 432344 (missing)

(geezmeister: "pseudo precipitation technique", Stimulants)

[SHORTY]

Thanks geez, shoulda known it couldn't bee that easy.  But it did feel good to bee motivated for a moment.

[Vaaguh]

So after the H2O/IPA/HCL was evaporated there was some lovely orange goo left, washing this goo with acetone gave a nice crystalline white powder, however the weighed crops where around the theoretical yield so that is a little bit too high for it to be all Pseudoephedrine Hydrochloride.

From what i understand freebasing would be unwise as there might be gak that can form a coating on the Pseudoephedrine Freebase

So later on the Geezmeister "pseudo precipitation technique" is going to be applied to get rid of the latest bit of GAK.

[geezmeister]

There was some lovely orange goo left, washing this goo with acetone gave a nice crystalline white powder, however the weighed crops where around the theoretical yield so that is a little bit too high for it to be all Pseudoephedrine Hydrochloride.

Whoa!

If you rinsed an orange goo away with acetone, and not just a yellowish tint, you may have done what we have been trying to do since January. If the orange is orange II gakk you may have cracked it with the hot HCl in the mix you boiled it in.

If you do the precipitation technique, how about slowly evaporating the xylene after extracting the pseudo and checking what might be in it?

[wareami]

Ibee has already cracked the RootBeerFloat gaak with the JD/TCE. YesindeedyPeaty!
Ibee has two bowls of blue tone rinses that contains the OrangeII gaak in the center! Orange as can bee!
The final tone washes are what attract it so, Yes, it is soluble in tone! The trick is to disarm it which is what the JD/TCE does! Then it readily cums over in the tone leaving the pfed behind!
Look for a new frontside solution to the blue here in comedycentral to bee posted momentarily!
Peace of the _reaction

Have FUN-Bee SAFE

[halfkast]

>>If you rinsed an orange goo away with acetone...

Thats what I was thinking.

I wonder if it is as easy as adding acetone to the aqueous solution, or concentrated acqueous solution.

Vaaguh you should hang around here as little as possible, your free thought may cease to exist...

And your initiative to add HCl was great I thought. I don't know how much you could add before it damages the sudo molecules though...

[geezmeister]

If the orange rinsed out with acetone, its been cracked and you are rinsing out the remnants that acetone would not have rinsed out before. That was the point I was making. HCl shouldn't be that much of a problem-- (if it were I would never have been able to a/b pseudo, as when I first started I used way, way, way more acid than I needed to.)  

Ware-- I hear you. I've done the same with JD in a naptha mix and JD in an MEK mix. It works with them and I assume it would with that stinky, smelly stuff you like to fool with. I much prefer to play with fire, myself. So to speak.     I think my attitude may be changing a little bit though. I seem to have developed an aversion to hot naptha I do not recall having had before.

[wareami]

>I wonder if it is as easy as adding acetone to the aqueous solution, or concentrated acqueous solution.

halfkast: More or less like a gaak vehicle? This might be possible if the aqueous solution isn't misible with the tone! These Orange gaaks aren't friendly critters and they don't play well with others. Beeing longchaingang patch warer's, they revel in yankin others chains! It's best to get them alone and then ya see what they're made of!

>And your initiative to add HCl was great I thought. I don't know how much you
could add before it damages the sudo molecules though...

Agreed wholeheartedly! Thare is such a thing as overkill. For that matter, underkill and straight UP MURDER!
There is a middle ground as in a quarter tern to the right or left.
"LOOK!!! UP in the sky, it's a plane, it's a tern, ......
it's a black helicopter!

>I seem to have developed an aversion to hot naptha I do not recall having had before.

Hot DAMN Bro!!! I certainly hope so! I'd hate to risk losing one of our own to ghet a point across! You know as well as others that Ibee's always strongly advised against heating solvents to a dangerous degree! This biz already has plenty of FLARE and enough built in showstoppers!
None among most bees are equipped to control vapor or it's unpredictability around switch spark when neither can bee seen!
And God forbid if one of those branchdudes starts shootin at the wouldshed when ya feel like heatin a cup of joe.... .......
Holy Fuck!!!! Hope Geez's name ain't JOE!
Peace of the _reaction

Have FUN-Bee SAFE

[halfkast]

Deer Geez & Ware,
Sorry ware I was thinking in freebase terms, I was thinking the acetone might break up the gels holding on to the pfed fb in solution.

I'm thinking he just rinsed away the remnants of the HCl wash.

I don't think orange is a part of the polymer that locks up the pfed. the hydrogels that lock up the pfed, the orange/brown is just an indicator.

swihk has seen the solutions, the hydrogel is visual way before the pH-of-pfed-migration is reached.

ware I've been wanting to know the name of the orange so I can try work out how you solved it with JD, tell me in PM if it's a secret.  

heh ware I'm sure geez knows you already cracked the "rootbeer".  

[geezmeister]

heh ware I'm sure geez knows you already cracked the "rootbeer".

Yep. I can tell from the length of the posts as well as the language. Something has happened to my brain though. I can almost understand that odd language without tequila these days. Hmmmm. Understanding Wareamiese without benefit of Tequila. Will wonders nevers cease?

[Vaaguh]

If you rinsed an orange goo away with acetone, and not just a yellowish tint


The residue that remained after evaporating of the solvents was orange to dark yellow, the acetone washes itself however where indeed of a dark orange color.


If you do the precipitation technique, how about slowly evaporating the xylene after extracting the pseudo and checking what might be in it?

There is only one problem at the moment i have no clue what otc product in this lovely part of europe has xylene in it, toluene is available however, would this make a decent substitute ?

In a couple of days i hope to have the time to do a TLC on some of the white powder that filtered out after the acetone washes, also i'm going to freebase some of the product and take a meltpoint to check if there is any pure PseudoEphedrine Freebase.

[Vaaguh]

After freebasing some of the PseudoEphdrine-HCl a white waxy looking freebase solid formed which i could not propperly filter by gravity filtration (it completeley clogged the filter) the freebase was turned back into the HCl and the h2o was evaporated the crystals where washed with ether.

The appearance of the just formed crystals had a more white look then the other PseudoEphedrine-HCl (both still contained some almost glass splinter like particles that glinstered, they are probably Silicon Dioxide aka Sand), washing the non freebased PseudoEphedrine HCl with ether did not gave these bright white crystals, a meltpoint of the non freebased PseudoEphedrine did also give weird results even over the 200 Celcius it did not decompose but just darken a little.

Initially the idea was to extract the PseudoEphedrine Freebase with ether but nothing went into the ether layer.

Perhaps some fluted filter paper would be nice to filter and wash the PseudoEphedrine Freebase with H2O, if this works it might give reasonable pure PseudoEphedrine HCl.