Need help.

[Bulldog44]

A friend of mine heard that some friend of his may try this RX soon. I'd like the crew to look it over as to its soundness. Then answer some of the questions in the post script.




RE: Simpler Oxycodone from Codine(ala Rhodium)"
 
   LAST EDITED ON 09-13-01 AT 00:35 AM (EST)
 
Hey you fuck heads: CODEINE --> OXYCODONE
Dissolve your codeine base in the acid solution(1) (acetic, we're following the method given at the begining of this thread somewhat so use those amounts) in a rb flask(2) and set it in an ice water bath with stirring(3). Now that it's nice and cool, slowly pipette in the dichromate solution.(12) The solution immediately turns a milky orange/yellow. Now remove the ice and set it in your oil bath on a hotplate and throw your water cooled condenser on top(4). I used a temperature controlled hotplate so I just dialed the temp in to ~83(5) and made sure it stayed there for ~20 min. If you stick a thermometer in your oil bath you should be able to do about the same. Heat is bad for opiates, but I have not found that letting it cook at 80-90 for 30 min. to be terribly detrimental. Anywayz, you can tell that the reaction is complete when there is no more color change. The new color should be a dark brown/red. Pipette pour your solution into a sep. funnel, wash your flask with a bit of water and pour that in too. There will be some black insoluble crap left in the flask. Don't worry about that shit. Now basify with ammonia.(6) You don't have to be exact, just make sure the pH is taken to above 10 and then extract three times with chloroform.(7) If you get an emulsion, just deal with it by adding a butload of chloroform and only taking the unemulsified chloroform with each separation. Take your chloroform solutions and back extract with water twice to make sure you didn't bring nasty Cr with your product. The product is yellow when disolved in a large amount of solvent and dark brown/red when concentrated. You just converted codeine's hydroxy group to a ketone and put a hydroxy under the nitrogen bridge. Evaporate off your solvent.(

BUYING Pd/C IS NOT ANY BIG DEAL BESIDES JOE BLOW IS ONLY GOING TO USE IT FOR LEGITIMATE PURPOSES SO HE HAS NOTHING TO WORRY ABOUT!!!!

Next is to reduce that double bond which is VERY EASY if you have a source of hydrogen. As far as other equipment, you need two syringes with the plunger removed and needles attached. To each you attach a balloon the the plunger end. Then, you need some sort of thick rubber to cover the mouth of your flask, but can be penetrated (air tight) by your needles. Ok, so you throw in like 3 molar %(of initial moles of codeine) of Pd/C (either 10% or 5% Pd on Carbon(9) into your flask which contains your goodies in a fairly concentrated solution of ~8% acetic acid in MeOH (Not super concentrated, but definately not super dilute)(10) with STIRRING. Then you fill your ballons through the needles, purge your flask air space with hydrogen by inserting both needles through the rubber diaphram and insert a third needle to allow an out flow. After it has purged for a while pull out the purge needle and make sure that the hole it created is now sealed. Refill your balloons and reinsert them. Let it stir overnight.(11) I have done this on a few gram scale so there wasn't a lot of hydrogen absorbed. If you were doing a tens of grams scale, you would need to refill the balloons several times during the reaction or you may still need to do this if you have bad leaks. Ok, so filter your solution. It's about the same color, maybe a little bit lighter, but don't worry cuz it worked. Again, basify, shake with chloroform and extract 3x. Evaporate, disolve in acetone and gas or drip in HCl to crystalize. Your crystals may turn to goo when exposed to air during filtration if you use wet HCl. Don't worry about it, just realize you are gonna have to drip an aqueous oxy solution into your nose instead of getting to snort bumps to get high. Do not over acidify during crystalization! When your solution turns from brown to clear, stop adding acid and filter. If you overacidify, your crystals will turn to brown goo balls in your flask. They won't be destroyed but if you dried and snorted 'em the leftover HCl's might burn your nose a bit.

This procedure is very easy and the whole shebang except for the work-up could be done in a day no sweat. The yields of both steps are very high yielding. I have taken an H-nMR of the compounds at each step of the way and found them to be highly pure with no observable starting material in their spectrums. So get to work! Next time I'll go over the conversion of oxycodone to oxymorphone which is super potent and this is even more simple of a reaction. None of the reagents in either synthesis are suspicious so fuckin' chill.


1.   What concentration is the acid and is it Glacial acetic acid.
2.   What’s an RB flask? Will a volumetric flash work?
3.   What doya do here, put the flask in a plastic tub filled with ice water then put both ontop of your stirrer?? Wouldn’t that interfere with the stirring action?
4.   If this is a reflux why would you need water? I have done cured refluxes with a balloon before. Is this the same thing? Would a condenser what without water ?
5.   I assume he’s talking Celsius.
6.   Can you sub sodium Hydroxide for the ammonia? Any hints on where I could find great OTC ammonia?.
7.   I can’t find a good outlet for Chloroform, can I sub DCM at this extraction step?and the last one also?.
8.   Is this Dihyrocodeine at this point?
9.   Ok I’m trying to understand MMOLS I just can’t seem to wrap my brain around it. Say your first RX is with 2 or 3 grams of Codeine. I could only get 1% PD/C. How much 1% PD/C will I need to add to the mix.
10.   The fluid is 8% acetic ace and Methanol. He says concentrated but not to much. What does that mean? I mean wouldn’t you just add  50ml of acetic and 50ml of Heet (methanol).
11.   OK I’m going to be using a small compressed gas cylinder with hydrogen in it. Pressure set to 35 PSI. I’m using a filter flask and running the gas line into the side vent. I’ve read about parr hydrogenation and stirring and shaking are defiantly different. Will this be dangerous to just leave the stirrer on overnight ?and will it work if just stirred?
       12.   I almost forgot is this sodium CR of Potassium CR
Thanks in advance for your help. Of course all is this fictional and for entertainment proposes only !!

[foxy2]

Have you read these?

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

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxycodone2.html

http://www.coldwaterworld.com/

http://leda.lycaeum.org/Documents/Codeine_FAQ.11309.shtml

all from Rhodiums Page, and there is more there

I hate my government, does this mean I'm a terrorist??

[foxy2]

"we're following the method given at the begining of this thread somewhat so use those amounts"

You need to reference the thread which this procedure came from!!!!!!!

I could UTFSE but I think its your job to make things easy for someone answering your questions.
I hate my government, does this mean I'm a terrorist??

[Bulldog44]

Gee Foxy I've been around the hive long enough to utfse and Rho is my home page. This is the simplist RX for conversion on the net. I've read all the threads and posts about this converson.With the help of some hive friends I successfully rx'd a nano of Meth. But I'm not really into gofast. I did that to get a feel for kicthen chemistry.

The amount of starting product  is 2 grams codiene freebase.

If you are any other chem God would help as in the past I'd appreciate it. And I did wake up in the midd;e of the night thinking that an RB flask is ROUND BOTTOM !!!! LOL

[neuromodulator]

Why bother to reduce the double bond with H2 over Pd/C in the first place?  Heroin and morphine have that double bond intact and they are quite active, right?

[Bulldog44]

Just trying to follow a good RX. You maybe right. This is for Oxycodone. I just wish I could get a few more answers. My friend is going to do the RX, but these un answered questions could mean the difference between good........and bad. When he did his Meth Nano it took about 5 trys. He really didnt care because 3 grams of stock cost 5 dollars....... now 2 grams of starting material is $ 100 dollars. HUGE DIFFERENCE !! I did read on Rho's site that some RX's don't use hydrgenation at all. That the pd/c and acid is enough. Any advice about this ?? is hydrogen really nesessary ?

[foxy2]

Well I am sure glad you read Rhodium page since the procedure you posted sucks ass and leaves out lots of details!!!
They were referenceing the second procedure on this page, dumbass.

https://www.thevespiary.org/rhodium/Rhodium/chemistry/oxycodone2.html

1. What concentration is the acid and is it Glacial acetic acid?

"30 grams of codeine in 80 ml water with 25 grams acetic acid"  So its approximately 25% w/w acetic acid or vol/vol since the density of GAA is 1.0490g/cm3.


2. What’s an RB flask? Will a volumetric flash work?
You figured this out on your own, impressive.
A volumetric flask should work but would most likely be a hassel and its not reccommended to heat a volumetric flask.  I would use the smallest visionware or equivalent glass pot(made for heating on stove) that you can find.  Or a small beaker should work for small batch dreaming.
 

3. What doya do here, put the flask in a plastic tub filled with ice water then put both ontop of your stirrer?? Wouldn’t that interfere with the stirring action?

No plastic won't interfere with your stirrer.  However you could stir by hand if you don't have a mag stirrer.  I woundn't use any metal pots or utensils, strictly glass or teflon if i was U. 


4. If this is a reflux why would you need water? I have done cured refluxes with a balloon before. Is this the same
thing? Would a condenser what without water ?

Ballon is only to contain gasses, in cured whatever you did.
I think this heating can be done without a condenser since the contents are not boiling.  See rhodium linked procedure.


5. I assume he’s talking Celsius.

Yes Celsius is the standard for technical discussions. Usually.


6. Can you sub sodium Hydroxide for the ammonia? Any hints on where I could find great OTC ammonia?.

Ammonia is at the store, get non sudzy.  You can concentrate the solution by doing something like Mr Clean does here, just don't condense the gas but pipe into the liquid ammonia solution.

https://www.thevespiary.org/rhodium/Rhodium/chemistry/birch.mrclean.html

7. I can’t find a good outlet for Chloroform, can I sub DCM at this extraction step?and the last one also?.

Substitution is probably ok, but opiates are much more fickel that simple molecules like meth or pseudo so?
Cloroform synth(glad your SO familar with Rhodium)

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

8. Is this Dihyrocodeine at this point?

No, it is 14-HYDROXYCODEINONE.(Again its great that you are so familar with the synths on Rhodiums page)
 

9. Ok I’m trying to understand MMOLS I just can’t seem to wrap my brain around it. Say your first RX is with 2 or 3 grams of Codeine. I could only get 1% PD/C. How much 1% PD/C will I need to add to the mix.

Look around more or read a tutorial on moles.  mmol is a millimole or 1/1000th of a mole.  By moles they probably mean moles of Pd.  Time to learn something, you will need this kind of knowledge if you hope to do more complex chem like what you propose here.  See sticky thread in methods forum for links to MOLE information.


10. The fluid is 8% acetic ace and Methanol. He says concentrated but not to much. What does that mean? I mean wouldn’t you just add  50ml of acetic and 50ml of Heet (methanol).

I think this means 8% GAA in methanol, no water in there at all.  The standard is weight/weight so 8% by weight GAA in methanol solution.


11. OK I’m going to be using a small compressed gas cylinder with hydrogen in it. Pressure set to 35 PSI. I’m using a filter flask and running the gas line into the side vent. I’ve read about parr hydrogenation and stirring and shaking are defiantly different. Will this be dangerous to just leave the stirrer on overnight ?and will it work if just stirred?

Filter flasks are NOT made for pressure, bee careful.  Vacuum is not equal to pressure. 
Vigorous(the faster the better) stirring should work just less efficiently that shakeing.


12.   I almost forgot is this sodium CR of Potassium CR

sodium dichromate(Gosh Rhodium comes in handy)

NoJailForPot

(http://www.nojailforpot.com/)

[Bulldog44]

Dearest Foxy,

  Thank you so much for taking the time and energy to answer my questions. I never said I was a genius, Just that I have done my research and I have read all the pertinent posts and sites.

 Just because I read something doesn’t necessarily mean I understand it. I ask the questions not to infuriate bees but to become a better kitchen chemist.

1.
Just a couple more questions and I’m sure my friend will be ready to try this.

The reflux question: one RX says reflux. One says just heat.
1.a
The solution immediately turns a milky orange/yellow. Now remove the ice and set it in your oil bath on a hotplate and throw your water-cooled condenser on top. I used a temperature controlled hotplate so I just dialed the temp in to ~83 and made sure it stayed there for ~20 min.

2.
The mixture is heated to 80°C with stirring until all the solid goes into solution; the temperature rises spontaneously to 90°C. After short standing, the base is precipitated from the cold solution as the dichromate by adding an The mixture is heated to 80°C with stirring until all the solid goes into solution; the temperature rises spontaneously to 90°C.

In your opinion which one is best ?? Would it increase yields to heat the mixture longer ?

I’d still like to know if Potassium Dichromate would be OK to sub for Sodium Dichromate.

I did find out the Ethyl Acetate or Dichlor would be an OK sub for Chloroform. I’m familiar with the making chloro at Rho’s site. It just seems to me to be as involved as the RX. I just didn’t want to make my own or buy some for $ 48 = 8oz


The RX calls for 5% PD/C. If I add more more 1% PD/C work  it work ??


The first sentence says the RX sucks. Care to elaborate on that ??in your opinion will it work ?? and if not what would you do with your 2 grams of codeine freebase and the above chems ??

Thanks again Sweety.