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WW4000
(Stranger)
09-10-02 13:11
No 354973
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extraction
of pfed from NEW sudafed tablets @look@
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COMMENTS
REQUESTED - please
Ok, here's what took place in a vision earlier today:
24 60mg sudafed dissolved in dH2O, filtered twice over through rock wool,
filtered then twice through filter paper (all 4 filterings using vacuum pump
and buchner apparatus). Resulting filtrate clear and orange.
Filtrate basified with NaOH until pH 13+, stirred, then extracted with
toluene. Toluene seperated off and put to one side in a beaker.
An equal volume of Toluene was made acidic by bubbling dry HCl gas steadily
through it until the Toluene fumed and became clear yellow.
Acidified Toluene added to freebase containing Toluene so as to precipitate
p-fed HCl. Combined Toluene's filtered thrice through a single disc of filter
paper (same disc each of the 3 times) and filtrate discarded. Filter paper
containing thin layer of pfed HCl then rinsed through with dH2O, with
crystals of pfed HCl then dissolving into that dH2O and down into the filter
flask.
Filtrate made alkaline as before with NaOH, then extracted with this time
DCM.
DCM allowed to evaporate in pyrex dish, affording long spindly clear crystals
of pfed freebase.
Now
then, these are the NEW sudafed which contain stearate/micro-crystalline
cellulose/etc.etc.
Would anyone dare to comment on the purity of these final (double extracted)
freebase pfed crystals? Who thinks that the crystals still harbour any 'Gak!'
?
[purple]comments greatly appreciated from this UK stranger
I AM A
UK BEE, FEEL FREE TO COMMUNICATE REGARDING SPECIFIC UK MATTERS
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acid_egg
(Hive Bee)
09-10-02 13:19
No 354978
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from
this UK bee.....
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.....naming sources is a no-no.
A
chicken is just an eggs way of making another egg.
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Ph0enix
(Stranger)
09-10-02 14:18
No 354993
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Interesting
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Seems simple enough.
No emulsions, wierd colors, or problems when you based the first time?
Quit teasing. You tell us.
I am
not prejudice rember also, I am not stupid first, also.
~Flinger~
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WW4000
(Stranger)
09-10-02 14:47
No 355008
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Initial
basifying of orange filtrate DID cause ...
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Initial basifying of orange filtrate DID cause cloudyness of the aqueous
layer, but very little of this crossed over into the organic layer. (Care was
taken when swirling the two layers in the sep. funnel so as not to create a
difficult emulsion, there is, I guess, a possibility that some pfed did not
make it over into the organic layer - as the two layers did not make
absolutely intimate contact)
Later, with the basification of the second water/pfed HCl solution, again the
water turned cloudy - but even after vigorous shaking with DCM in the sep.
funnel, no emulsion formed and the DCM remained perfectly clear.
Does any bee have anything negative to say about this all.
What with the new extraction procedures outlined by Fester with his
'steam-cooker' it seems too straight forward to get clean pure pfed freebase
this way????
I AM A
UK BEE, FEEL FREE TO COMMUNICATE REGARDING SPECIFIC UK MATTERS
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BenWiFFen
(Line Monitor)
09-10-02 16:30
No 355053
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Not
playing with the same
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Not playing with the same brand but I fill h20 is not the best thing to hit
it with. The method that has ben working good around this cave. Toss the
babies in a tall jar add alc of choice after awile they will disolve
sometimes a tad of heat with some smashing but not always just stiring works.
Let set atleast one hour or until clear sep and evap slow. Then add
used toulene (n/p) and bring to a boil to rid any orange this is done atleast
three times until no more orange is noted. Then a hot acetone rince or two
will rid any green. Doc Suess would turn over in his grave. This doesn't work
on all pill as we know. No fuss no muss that you don't need.
What
good is your ride without a FAT gear box ???
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zibarium
(Naked)
09-10-02 17:27
No 355095
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sounds
cool; but what about yield?
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without a yield comment; much less a post rxn bio-assay comment from you,
how can one bee expected to respond?
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acid_egg
(Hive Bee)
09-11-02 15:14
No 355406
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further...
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Also a list of all the inactives would give a better idea of things.mcc and
stearic acid or salts don't count as gak of any significance.
A
chicken is just an eggs way of making another egg.
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geezmeister
(Bee of the Month)
09-11-02 15:26
No 355407
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I
don't know, but
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I would not be surprised if the extraction method let polyethylene glycol
carry through with the crystals. You could have extracted the freebase
crystals and lost it, but if it were present in the pill to start with, this
technique would not get rid of it. My thoughts, anyway. Don't know which
tablet you used or whether PEG was in it. It it had PEG in any significicant
quanitity, you should recrystalize your crystals in bone dry ISO OH and dry
acetone to shed any PEG that might be there.
Of
counsel. On Tuesdays.
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WW4000
(Stranger)
09-12-02 13:22
No 355684
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the
inactive ingredients are as follows...
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firstly, thankyou for the replys that those of you have made to my original
post.
here follows the list of tablet ingredients as per the enclosed
literature....
pseudoephedrine hcl 60mg
lactose
micro crystalline cellulose
maize starch
silica
magnesium stearate
hypromellose
polyethylene glycol (aarrghh the PEG)
talc
red iron oxide
These are what you get OTC in the UK currently (they were different in 1997)
Hopefully these particular tablets do not require the pressure cooker method
ww4000
I AM A
UK BEE, FEEL FREE TO COMMUNICATE REGARDING SPECIFIC UK MATTERS
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geezmeister
(Bee of the Month)
09-12-02 13:28
No 355687
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soak
'em first
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A presoak in xylene or tolly will get the PEG out. Or do an extraction
process even easier than the one you followed--VideoEditor's "Straight
to Bee"-- and take Cthulhujr's advice about redissolving the freebase
crystal in fresh non-polar solvent before titrating to get the salt form. Or
do a freebase reaction. Great results.
Right now, no need to reinvent the wheel. Until they figure out how to wreck
the ones we have, anyway.
Of
counsel. On Tuesdays.
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geezmeister
(Bee of the Month)
09-14-02 06:03
No 356262
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or
then again
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I was thinking about the technique you used and realized that as you
introduced the HCl in tolly without water being present, you may have avoided
the PEG. I am uncertain whether the PEG will follow through with gassing or
with the technique you used. IT will follow through if there is any moisture
available when the HCl is introduced. Whether it followed through on your
technique would be nice to know. The introduction of the HCl gas to the tolly
and mixing that tolly with the tolly containing the freebase may be a way
around PEG this geezer has not considered.
What were your results? Did the pseudo recrystalize cleanly or was there some
mucus-textured white stuff that fell out on dissolving with dry ISO OH?
This bee would like to know.
Of
counsel. On Tuesdays.
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WW4000
(Stranger)
09-14-02 08:31
No 356279
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end
result at last
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this seemed to work fine...
single pack of 24 dissolved in dH2O, filtered twice through rock wool, then
twice through filter paper (all times with vacuum), filtrate basified and
freebase extracted with DCM, equal volume of pre-acidified HCl DCM added to
freebase DCM - stirred well - then all DCM evaporated leaving decent p-fed
HCl crystals.
Notice how in my original post it was the freebase form of pfed which was the
final result? Well that was an error on swiw's part, as it was actually the
HCl salt that was called for for making the acetic ester followed by NaBH4/Pd
reduction/hydrogenation.
So, basically the above extraction procedure works fine for UK current brand
name 24's
NOTE: The end product meth HCl was green? The 'octane' rating was not amazing
unfortunately (perhaps something to do with not razemising the pfed first? or
having the less favourable [d], or [l] , havent quite got head round that
business yet.....
ww4000
I AM A
UK BEE, FEEL FREE TO COMMUNICATE REGARDING SPECIFIC UK MATTERS
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