i need help with demethalating codeine

[daxium]

dude, swid is having some tough luck here swid does the reaction (codeine freebase with pyridine hcl) everything seems to be fine swid filters extracts w/ chloroform and adjusts the ph and do i get morphine to seed out, of course not??? any sugestions?

[Rhodium]

https://www.thevespiary.org/rhodium/Rhodium/chemistry/codeine2morphine.html

[daxium]

i tried using the "homebake" method and i never got any morphine to precipitate out what am i doing wrong? I am using ammonium hydroxide not sodium hydroxide to raise the ph, extract w/ chloroform and lower the ph to 9 filter and lower it to 8.5 and try to get chrystals nothing precipatates, what the fuck am i doing wrong here???

[SPISSHAK]

And Ammonium hydroxide won't form a alkali phenolate salt with morphine.
Sodium Hydroxide will.
This may mean that during your workup you co-extracted morphine along with your unreacted codiene.
Also if you look at some of extrraction patents they mention diiferent ways to precip morphine by the addition of different salts to the aqueous mother liquor.
I'll look it up.

[daxium]

i'll answer the part about more specific when i know what to be specific about. i extracted with chloroform to get out the unreacted codeine and when the chloroform was evaporated there was nothing in it no unreacted codeine or anything at all almost only just a pussy hair of powder. i don't have any sodium hydroxide right now and i was thinking that the hydroxide ion is the part that changes the ph and that is what i want to do but you may be correct on the sodium ion making the correct salt to precipate out any wat if you can get the info on getting the morphine to precipate out that would be great so hopefully you can help me out here

[SPISSHAK]

I mean the equipment you used, the ratios of reactants, etc. For example how did you check the PH?
Morphine is PH sensitive so you may have preciped out the crud and the morphine at the same time.
Also, how did you monitor the temperature?
If your temperature was'nt accurate that could have some implications as well.
Also what form of codiene did you use, how was it worked up?
Purity plays a role in reactions.
That patent I'm still looking for,but basically it's the same principle as salting out a compound from a mother liquor, what happens is the salt nuetralizes the charge keeping the compound suspended so it precips.

[ClearLight]

Morphine has a really weird pka ~ 10.  At pH 10, only 20% or so will come across in the organic solvent... your much better off forming an hcl or just freebase at ph4 or 5 and having the org layer suck off all the crap.  check up on how the opium boys do it, they've got it down and it's ghetto simple when you understand that by and large, morphine is not soluble in an organic solvent.

Infinite Radiant Light - THKRA

[daxium]

The codiene was pure freebase extracted from tylenol and asperin #1's with codiene, pure white powder. i used an oil bath that had the temp at 250 degrees so the temp was hot enough, i added the pyredine hcl (3 grams)to the test tube and melted it in the oil bath then quickly added 1.5 grams codiene freebase and stoppered it with a stopper wrapped in filter paper, heated it in the oil bath for both 3 min, 10 min, and 14 min. added this to 50 - 60 mls h20 and basefied with ammonium hydroxide to ph 14 then extracted twice with about 25 mls chloroform, changed to ph 9 filtered and lowered to ph 8.5 with dilute hcl and no morphine would precipitate out i tried the seeding stick method with no success. i used narrow range ph paper to test the ph. when i look at the patent it removes the sludge and morphine at the same time and then adds them to methyl hydrate and filters to get the morphine disolved in the methyl alcohol. I am wonedring if anyone has personal experience with this for there help please

[SPISSHAK]

You used narrow range ph paper?
If it gave an incorrect reading you could have preciped morphine too.
PH strips can be a little inaccurate sometimes.

[daxium]

that is possible, but didn't you say that i needed sodium hydroxide and not ammonium hydroxide? the ph papers are kind of a bitch but they do seem pretty accurate the only thing is that the ph changes so weiredly somtimes and i would pass the correct ph and have to fix it with more ammonium hydroxide, anyway after doing the reaction and mixing with water what would you suggest for getting the morphine out in a patent it sugests getting the junk and morphine out at the same time and using methanol to get the morphine out???    HELP!!!!!

[Rhodium]

After each addition of acid or base, wait at least 1-2 minutes (with good stirring) before testing. The pH change may not occur instantaneously.

[SPISSHAK]

Is a method of recrystallizing morphine base from alcohol.
Try it, what do you have to lose?
I haven't seen the patent your'e talking about so I don't know but try recrystallizing the gunk you precipitated from an alcohol.
Or take it up in aqueos NaOH and start over.
With the phenol seperation.
But I would try the recrystalizing first, if it doesn't work, the evaporate the alcohol and use the aqeous phenol seperation, you know the principle behind this don't you?

[daxium]

before the homebake method where they filter the junk and the morphine out together and then disolve it all in hot methanol then filter the methanol and re-chrystalise the morphine from the solution that should filter out most of the junk read the method that is the first one on the link rhodium provided in the begining of this thread. also i don't know what you mean by "aqeous phenol seperation"

[gamilaraay]

[SPISSHAK]

To answer your question aqueos phenol seperation involves the formation of an alkali phenolate salt.
This makes it water soluble while non-phenolic compounds are seperated by means of solvent extraction, or filtration.
Then the phenol is made hydrophobic by titrating the solution and neutralizing the alkali phenolate salt with acid.
This is the procedure they use to precipitate morphine since it bears a phenolic hydroxy function in the 3 position, hence a phenolic compound.

[wirringun]

 i am not an academically trained chemist
 but SWIM has followed rhodiums codiene 2 morphine review
 with some joy 'home bakemethod'resulted beige color product
 SWIM followed exact specs and no trouble
 maybee the change from using sodium hydroxide to potassium
 maybee the key ,like i said im not a chemist but im sure i
 heard that potassium hydroxide destroys the phenolic    
 matreial .like i said im not  CHEMIST
listen to spissak fella he seems to know whats going on follow specs EXACTLY
cheers hope you have more luck
peace
wirringun