Author Topic: Hydriodic acid codeine reduction purification?  (Read 188 times)

hyjroul

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Hydriodic acid codeine reduction purification?
« on: January 21, 2013, 10:51:31 PM »
What do you do if you have 3g of codeine base and I/RP, ratios? And when reduced use the post-reaction method as with meth ? Not making shit krokodil injectable liquid, I want for smoking on foil.

regards

theimport2012

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Re: Hydriodic acid codeine reduction purification?
« Reply #1 on: January 22, 2013, 04:19:25 AM »
Can you steam still it. If not just go and  base to a ph of 10 (na2co3)  and acidify to 7 check the ph of the base first but swIM thinks its not as high as MA. Just a guess but :) Sure it would work.

atara

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Re: Hydriodic acid codeine reduction purification?
« Reply #2 on: January 22, 2013, 05:29:21 PM »
What do you do if you have 3g of codeine base and I/RP, ratios?

While this isn't the real mechanism, the pseudo-reaction is
HI + codeine -> morphine* + CH3I
HI + morphine -> iodomorphine + H2O
HI + 6-iodomorphine -> 6-desoxymorphine + I2
HI + 6-desoxymorphine -> 8-iododesomorphine
HI + 8-iododesomorphine -> desomorphine + I2
3I2 + 2P -> 2PI3
PI3 + 3H2O -> 3HI + H3PO3
which is fine for stoichiometry purposes. Now go learn some math. :)

*morphine cannot be extracted from this reaction, sorry
« Last Edit: January 22, 2013, 05:31:09 PM by atara »

Sedit

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Re: Hydriodic acid codeine reduction purification?
« Reply #3 on: January 23, 2013, 06:00:30 PM »
What do you do if you have 3g of codeine base and I/RP, ratios? And when reduced use the post-reaction method as with meth ? Not making shit krokodil injectable liquid, I want for smoking on foil.

regards


Reduced? Your not trying to reduce anything your trying to cleave an Ether. This can only end badly.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

hyjroul

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Re: Hydriodic acid codeine reduction purification?
« Reply #4 on: January 24, 2013, 01:22:44 PM »
I was high. xD

I mean, if you  do the ''russian'' desomorphine synth, but well calculated and carefully made (in a lab) and then extract the desomorphine base for smoking, how much will be the yield?

Also it's suitable  the use of anything more OTC than boron trihalides to O-demethylate codeine in high yield?

regards

fractal

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Re: Hydriodic acid codeine reduction purification?
« Reply #5 on: January 24, 2013, 02:58:34 PM »
Pyridine HCl works, you can find this and more information on rhodium. UTSE.
« Last Edit: January 24, 2013, 06:33:30 PM by fractal »

hyjroul

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Re: Hydriodic acid codeine reduction purification?
« Reply #6 on: January 24, 2013, 03:32:34 PM »
I said HIGH-YIELD O-DEMETHYLATION (80%+) I think pyridine it's only 15-30% not worth the trouble..


What is the  average yield for well-done HI + codeine ---> desomorph synth?

Doesn't HI transform the codeine into apomorphine?, i read somewhere that codeine + strong acids will yield emetic apomorphine shit

regards!! :)


fractal

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Re: Hydriodic acid codeine reduction purification?
« Reply #7 on: January 26, 2013, 11:54:53 AM »

hyjroul

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Re: Hydriodic acid codeine reduction purification?
« Reply #8 on: January 27, 2013, 04:41:39 PM »
Yeah I read lots of posts in demeth. of course but i'm wondering about the conversion of codeine into desomorphine, not o-demethylation specifically in this case!


And about the demethylation , getting BBr3 it's almost impossible and it's very fucking expensive, anyone knows a way to get cheaper BBr3 o other boron trihalide to get the high yielding shit? as I said in earlier post.

I reask, anyone know if the HI ether cleaving of the codeine , if done well will yield desomorphine in realitve high-yield (at least 50% ? ) and if it can be purified into pure desomorphine base or HCl, all info is very appreciated, I will dream this as soon as i get a good reply and posts the results on here.

Regards!! :)

Assyl Fartrate

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Re: Hydriodic acid codeine reduction purification?
« Reply #9 on: January 27, 2013, 11:09:07 PM »
Desomorphine via HI generated in situ from P and I2 is a flat out bad idea. The crude is a complex mixture that is difficult to resolve, the yield of the desired product is low, and there's no easy way to clean it up - acid/base extractions are out, as desomorphine is amphoteric (and so are many of the side products), and any recrystallization carries the risk of co-crystallization of impurities and loss of a substantial amount of material. The only good way to clean up a mess like what this reaction provides is to run a column, and not many clandestine chemists have such resources, or even the experience necessary to do such a thing.

Try a Birch on codeine. Li/NH3 reduces allyl alcohols quite cleanly and selectively, so it'd probably give you desocodeine, which, given studies on structural activity relationships in opiates, should be fairly potent (not so much as desomorphine, but improved yields should make up for it) and have high oral bioavailability. This isn't amphoteric, so it could be cleaned up with an acid/base extraction. The possibility of ingesting extremely toxic phosphorus compounds would be avoided entirely.
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hyjroul

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Re: Hydriodic acid codeine reduction purification?
« Reply #10 on: January 28, 2013, 12:26:01 PM »
I thank you a lot that Assyl Fartate as I have experience in Birch reductions , I will investigate more in the desocodeine. Do you think it is smokable?

And do you know any other powerful compound ''easily'' synthesized from codeine to investigate ?


Thank you a lot all and sorry for my relative poor english!! :)

Assyl Fartrate

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Re: Hydriodic acid codeine reduction purification?
« Reply #11 on: January 28, 2013, 04:56:23 PM »
Esters of 14-hydroxycodeinone would fit the bill there. 14-Cinnamoylcodeinone is approximately 180x morphine, and can be prepared in three straightforward steps from codeine: first, MnO2 (prepared in a specific manner) or another reagent capable of converting codeine into codeinone is used to effect said transformation, then catalytic aqueous CuSO4 or MnSO4 is employed to oxidize codeinone to 14-hydroxycodeinone using atmospheric oxygen, and finally this is hit with cinnamoyl chloride or bromide to generate the ester.

There are many other possibilities that begin with codeine, but this is probably the easiest. Search for posts by "Assyl Fartrate" and throw in terms like "morphine," "oxycodone," "oxymorphone," "codeine," "fentanyl," and "analog" and you may find some summaries of ideas formerly posted. Also search for posts by "jon" as he is our resident medicinal chemist and his knowledge in this area is considerable - he has contributed greatly to the pursuit of the goal of easy opioid synthesis in a home environment.

If you are actually serious about pursuing one of these syntheses, Assyl will walk you through the process, given that you have accepted a gentlemen's agreement that you will stick around to share your experiences with the end product.
« Last Edit: January 28, 2013, 05:00:58 PM by Assyl Fartrate »
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hyjroul

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Re: Hydriodic acid codeine reduction purification?
« Reply #12 on: January 28, 2013, 05:38:29 PM »
Obviously yes, I will share all my experiences of everything here, I'm very interested in doing this kind of things, I haven't got too much of space in my ''lab'' but as soon as my money permits me I will update my lab , althought not much 'real' experience in advanced chemistry I decided to change my studies so I currently started my ''formal'' chemistry classes I started in September so i'm learning little by little I hope in a couple years have at least a cool space to work, I'm a south european bee by the way ;)

Thank you Assyl Fartate for you replies I will keep investigating on opioid chemistry!

Regards!! :D