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oxycodone synthesis 14-HYDROXYCODEINONE: Thesame product obtained from the 30% hydrogen peroxidetreatment of thebaine in acetic acid can also be obtained directlyfrom codeine.30 grams of codeine in 80 ml water with 25 grams acetic acid, is

treated cold with a solution of 20 grams sodium dichromate in25ml water. An oily precipitate forms which becomes crystalafter short warming. The mixture is heated to 80C with stirringuntil all the solid goes into solution; the temperature risesspontateously to 90C. After short standing, the base isprecipitated from the cold solution as the dichromate by addingan excess of chromic acid solution. Crystallize from alcohol witha little chloroform as plates, decomposes at 275C. Stable tostrong acid or alkali. Soluble in chloroform, ethyl acetate, ligroin.Sparingly in alcohol, insoluble in ether or water.Simple hydrogenation over Pt, Pd, or Ni would satutate the

recovered and purified compound to the potent dihydro version.Hydrogenation over Pt or Pd in dilute acetic acid give 93% to97% yields. This product would be 14-hydroxydihydrocodeinoneor Oxycodone, either as the dichromate or possibly acetyl salt.What I like about this procedure is that it is simple and fast anduses only very available reagents.What I don't like about it is that no yields are stated.Codeine -> 14-HydroxycodeinoneDissolve your codeine base in the acid solution (acetic, we'refollowing the method given in Lone Ranger's procedure above,

so use those amounts) in a rb flask and set it in an ice waterbath with stirring. Now that it's nice and cool, slowly pipette inthe dichromate solution. The solution immediately turns a milkyorange/yellow. Now remove the ice and set it in your oil bath ona hotplate and throw your water cooled condenser on top. I useda temperature controlled hotplate so I just dialed the temp in to~83C and made sure it stayed there for ~20 min. If you stick athermometer in your oil bath you should be able to do about thesame. Heat is bad for opiates, but I have not found that letting itcook at 80-90C 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. Pipettepour your solution into a sep. funnel, wash your flask with a bitof water and pour that in too. There will be some black insolublecrap left in the flask. Don't worry about that shit. Now basifywith ammonia. You don't have to be exact, just make sure thepH is taken to above 10 and then extract three times withchloroform. If you get an emulsion, just deal with it by adding abutload of chloroform and only taking the unemulsified

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chloroform with each separation. Take your chloroform solutionsand back extract with water twice to make sure you didn't bringnasty Cr with your product. The product is yellow when disolvedin a large amount of solvent and dark brown/red whenconcentrated. You just converted codeine's hydroxy group to a

ketone and put a hydroxy under the nitrogen bridge. Evaporateoff your solvent.14-Hydroxycodeinone -> OxycodoneNext is to reduce that double bond which is VERY EASY if youhave a source of hydrogen. As far as other equipment, you needtwo syringes with the plunger removed and needles attached. Toeach you attach a balloon the the plunger end. Then, you needsome sort of thick rubber to cover the mouth of your flask, butcan be penetrated (air tight) by your needles. Ok, so you throwin like 3 molar % (of initial moles of codeine) of Pd/C (either10% or 5% Pd on Carbon) into your flask which contains your

goodies in a fairly concentrated solution of ~8% acetic acid inMeOH (Not super concentrated, but definately not super dilute)with STIRRING. Then you fill your ballons through the needles,purge your flask air space with hydrogen by inserting bothneedles through the rubber diaphram and insert a third needle toallow an out flow. After it has purged for a while pull out thepurge needle and make sure that the hole it created is nowsealed. Refill your balloons and reinsert them. Let it stirovernight. I have done this on a few gram scale so there wasn'ta lot of hydrogen absorbed. If you were doing a tens of gramsscale, you would need to refill the balloons several times duringthe reaction or you may still need to do this if you have badleaks. 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, disolvein acetone and gas or drip in HCl to crystalize. Your crystals mayturn to goo when exposed to air during filtration if you use wetHCl. Don't worry about it, just realize you are gonna have to dripan aqueous oxy solution into your nose instead of getting tosnort bumps to get high. Do not over acidify duringcrystalization! When your solution turns from brown to clear,

stop adding acid and filter. If you overacidify, your crystals willturn to brown goo balls in your flask. They won't be destroyedbut if you dried and snorted 'em the leftover HCl's might burnyour nose a bit.This procedure is very easy and the whole shebang except forthe work-up could be done in a day no sweat. The yields of bothsteps are very high yielding. I have taken an H-NMR of thecompounds at each step of the way and found them to be highly

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pure with no observable starting material in their spectrums. Soget to work! Next time I'll go over the conversion of oxycodoneto oxymorphone which is super potent and this is even moresimple of a reaction. None of the reagents in either synthesis aresuspicious so fuckin' chill.