Opioids Rikodeine acid base extraction

[Like dead]

Yes, I know, this has been covered a million and one times, yet there never is a conclusion. Someone always says: do an acid base extraction. Sometimes they post a procedure for morphine syrup, which is VERY different from DHC because freebase morphine is practically insoluble in water, whereas freebase DHC is supposedly quite soluble.

My questions are: has anyone tried this?
What is the solubility of DHC freebase in water?
Is toluene an appropriate solvent?
What is the solubility of DHC freebase in toluene or appropriate non polar solvent?

Will this procedure work: shake the syrup (lightly, emulsions suck) with your non polar solvent to rid the soluble substances which we don't want. Repeat this untill the solvent comes out clean. Discard or set aside for distillation (for reuse).

This is where I'm unsure. I remember some source saying that 1g DHC freebase is soluble in 200ml water. Rikodeine contains 19 mg per 10 ml. That's 380mg per 200ml. Does this mean that when I basify the DHC base will dissolve in the water and never migrate to the non polar solvent? Please explain this. If this is so, the majority of water needs to be evaporated off. What heat is safe and how sensitive is DHC to heat exposure.

Now add a sufficient amount of non polar solvent to dissolve DHC base. Base to between 9.5 and 11.5 PH with sodium hydroxide or ammonium hydroxide. Shake, seperate repeat with new solvent. Mix the non polar solvent (now containing DHC hopefully) with water and acidity to below 5ph. Slowly evap off water.

If this will not work or if you have any suggestions please post them
thanks in advance.

 

[Like dead]

Oh, does anyone know If there are any OTC solvents with which I could form a low boiling water azeotrope? I'm not sure what the bp of acetone water is but I'm considering that.

 

[JamtasticX]

I'm not really sure, however I found this post which might help. This was for morphine syrup, however, I believe you should be able to do it with DHC Rikodeine

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You will need a gallon of distilled water, an amount of non-polar solvent in twice the amount of your morphine syrup, a pH meter, seperating funnel, a very small amount of hydrochloric acid,and a tiny amount of sodium hydroxide in a 10% formulation. All these things are relatively inexpensive and easy to obtain.


Now, the "recipe":I] Take your syrup and combine it with an equal amount of the distilled water.

II] DROPWISE, add your 10% sodium hydroxide until the pH hits 11.5 .

III] Add your non-polar solvent [DCM works fine] in an amount equal to your COMBINED distilled water and syrup and combination.

IV] Add it all to your seperatory funnel and agitate moderately for 5 minutes.

V] Let stand until it separates into distinct layers.

VI] Remove the water layer [the top layer which will be lighter in color, etc.].

VII] Add an amount of distilled water equal to the removed water layer.

VIII] Agitate for 5 minutes, moderately.

IX] Let stand until it separates, as before in Step V.

X] Repeat Step VI again.

XI] Repeat Steps IV, V, VI, VII, and so on another 3 times

XII] Now add an amount of distilled water equal to the amount of non-polar solvent used.

XIII] Again, let stand to separate.

XIV] Add hydrochloric acid DROPWISE until you hit a pH of 9.1 .

XV] Let is stand to separate.

XVI] Evaporate to get to the goodies, morphine hcl.



Notes: You want to be sure to repeat the cumbersome agitate, let stand, separate" steps above becuase the if you do not remove all your sodium hydroxide it will react in a bd way [understaement] with your hydrochloric acid].

If you are just satisfied with a liquid morphine freebase you can simply stop after Step XI. If you follow through, and fully evaporate, you will have a pretty nice morphine hcl. Good luck.

Source:http://www.bluelight.ru/vb/showthread.php?t=331789

 

[Like dead]

As I said before, I think since the solubility is significantly different (I think), it may not work on DHC. Thanks for posting though. Still considering the azeotrope thing. Could do a turpentine wash, form and azeotrope and evaporate down to 10 ml or so, then do an A/B extraction? Anything which will give me the DHC in powder form. Fucking disgusting syrup, I wished they still had the aspirin DHC tabs or the English paramol.

 

[Ohwhatfun]

This site never gets boring I thank this post!