...is this the writeup you're referring to Rhodium and LT?
SIEGFRIED'S FENTANYL SYNTH REWORK by OZZA
THIS is a clear cut (every day chemists) guide to Fentanyl synthesis, adapted from Seigfried's Fentanyl synth - RHODIUM'S PAGE, which in my opinion is 50% correct. My adaption is a clear cut, updated format that cuts through all the crap and talks in "real time".
"Fentanyl synthesis re-visited & re-hashed"
For this synth, you want to use no smaller than a 3-neck-2000ml rb flask and up.. trust me. Any time I mention heat, its done with a mag/hot plate stirrer with an oil bath of peanut oil.
1- 25 g of 1-(2-phenethyl)-4-piperidone (also known as N-phenethyl-piperidone-4) is mixed with 60 ml aniline until dissolved. The 3-methyl analog requires N-phenethyl-3-methyl-piperidone-4 and the alpha analog uses N-(2-phenylpropyl)-piperidone. The para-fluoro analog could also be made, by using para-fluoro aniline, but the purification process would have to be altered.
2- 10 grams of 4a molecular sieves are added slowly and the whole mix is stirred (slowly), for 24 hours, at 60 deg cel.
3- The sieves are filtered out of the mix, with a coarse filter, to just remove the sieves.
4- The sieves are washed with 20ml tetrahydrofuran, to get all the mix off them. You can wash twice if this isn't enough. Add this wash to the shite you've just filtered.
5- Take the mix, less the sieves, and add 200ml anhydrous methanol. Give it a good stir, with your mag stirrer, for a few minutes.
6- 15gms of NABH4 are added very slowly ('cause if ya don't your gonna get the mix jumping right out of your flask!)...sooo add about 1gm at a time until the bubbles and foam go down to a level you can deal with. When all is added, stir the mix for about 4 hours at room temp.
7- Now connect the flask to a vacuum distillation set up and distil off the THF and methanol. Be careful not to over heat or burn it. The slower the better. You don't have to evaporate until completely dry cause it will most likley burn it. Just distil until there is a thick sludge at the bottom of the flask.
8- Add 500ml h20 to the flask and sludge. Start up the mag stirrer and start stirring the crap out of it. Add 20ml 35-37% hcl (muriatic acid)...(it really smokes so watch it and don't breath the shit).
9- A thick brown/red oil will form on the top of the h20. Keep stirring for a while until all the oil is on top. Next let it sit...until all of it is on top. (this oil is what you want)
10- Seperate the oil with a sep. funnel or just poor off the h20 and oil carefully. Collect the oil.
11- Toss the rest... keep the brown/red oil.
12- Take the oil and add 80ml pyridine. Stir at room temp or just warm a little if it helps the mix process. Stir for 4 hours.
13- When completely mixed add 77ml propionyl chloride (this shit really stinks and will knock you on your ass so be careful and wear a gas mask or use a good fume hood).
YOU HAVE TO ADD THE PROPIONYL CHLORIDE VERY VERY SLOWY! ..just a few ml's at a time. Before you start, add a thermometer to the flask set-up, because you CAN'T PASS THE 60 DEG C MARK. This is exothermic.. meaning when you add the prop.chlor. it is going to GET REAL HOT all by itself from the chemical reaction. So sit back and add LITTLE BITS VERY SLOWY. During this addition you are still stirring the mix with the mag stirrer.
Add it all then stir for 12 hours at room temp.
14- Your gonna have some nasty looking sludge in the bottom of the flask. That's good.... thats what you want .... now....take 250 ml of muriatic acid (hcl) 35/37% and put it into a seperate 1000ml plus flask. Add 750ml h20. Mix this h20 acid mix and then dump it into the flask with your sludge in it. Immediatley get that mag stirrer going at full tilt. There will be a lot of thick sludge chunks in the mix that are going to take some good stirring to dissolve. Turn on your oil bath at this point to warm the solution. This makes the sludge dissolve a lot easier.... Continue heating and stirring for another 12 hours. You gotta get all that shite dissolved.
15- Now take all the mix and wash it with 200ml ch2cl2 (dichloromethane). Do this twice. This means you need a huge flask or container unless you want to divide it up in smaller parts....anyway you take the acid/h20 sludge mix and empty it into a 2000ml plus flask and then add 200ml dichloromethane and put a lid on it. SHAKE THE HELL OUT OF IT for a good 30 seconds and then let it seperate before you do it again. The stuff you want will be at the bottom in the dichloromethane, which is now brownish. Pour off the water and put the dichloromethane mix in a seperate flask, then repeat this step, adding the dichloromethane to the first batch when done.
16- Now distill off the dichloromethane under vacuum and you will have a thick reddish brown oil. This is your pure fentanyl. Again be careful NOT to over heat when vac. distilling!
17- When NO more dichloromethane comes over, stop the distillation. Let the oil cool for a few hours or just cool it in the sink with some cool h20. When cool, add 200ml of acetone to the flask and swirl the mix for about 5 minutes. The fentanyl hcl will drop out of the acetone, meaning you will see a powder form and start sinking to the bottom .... Let this play out for a few minutes and then filter out the powder. Put the liquid in a flask in the freezer.
This way,if anymore "falls out" you can get it later...Take the filtered powder and spread on a pyrex baking dish. Warm gently, chop and mix...... chop and mix...... To let *ALL* the acetone and solvents evaporate off.
18- When totally dry, you will have roughly 15.5 grams of pure fentanyl hcl.
19- As I'm sure you know by now, YOU CANNOT USE OR SELL THIS IN THIS FORM...AND IF YOU DO YOU WILL HAVE MORE DEATHS ON YOUR HANDS THAN PROFIT!
20- To remedy this....and cut it properly....take 15.5 grams of your product and dissolve in 200ml methanol.
21- Then take 300 gms or roughly half a pound of "lactose" (get it for $4.00 per pound at any health food store). Spread the lactose out on a glass baking sheet and then add dropwise the methanol mix. Then mix it up thouroghly and then when mixed .....put in oven...bareley warm and heat and mix, heat and mix......You have to put in a lot of time mixing this shite so BE PATIENT!!! When dry (make sure you break up the rocks and mix very well) you will have a light brown/yellow to whitish powder that is 50% stronger than the "black-tar" dope on the street from Mexico...or even much stronger than Chinese or Burmese white dope. All this weaker dope is "organic-dope" or diacetyl-morphine that has been synthesized from the opium poppy (papaver somniferum). It is *NO* match for this "SYNTHETIC HEROIN".....At this ratio the amount will be over 1/2 pound of dope....The other chemists recommend adding *ANOTHER* 1/2 pound of lactose to the mix (to make it over 1 full pound) cause it is VERY VERY VERY VERY STRONG .With just a 1/2 pound of lactose, your gonna have dope that's 50% stronger than the *STRONGEST* street dope.......so you be the judge. No matter what you do......you still have to add that first 1/2 pound of lactose....'cause there is no way your gonna be-able to bag and sell the pure fentanyl with out killing a lot of customers. If you add one full pound of lactose to the 15.5 gms of pure fentanyl hcl..... you will have the same potency as "good" black tar or any "good-qaulity" diacetylmorphine.
**SYNTHESIS OF N-PHENETHYL-4-PIPERIDONE**
-Use at least 2000ml round bottom three neck flask for this synthesis.
-Also needed is one 76mm cel. thermometer
-Thermometer adapter
-Magnetic stiirer/hot plate
-Magnetic stir bar/egg or cross(large)
-Oil bath (peanut oil rec.)
-Reflux/condenser (water cooled)
-Sep. funnel or addition funnel
-Distillation condensor (water cooled)
-Vaccuum adapter
-Vaccuum pump with a minimum 29hg rating
-Chemical resistant tubing (to connect vaccuum to glassware)
-Fume hood or proper rated gas mask or enclosed breathing apperataus
-1000ml plus "receiver flask" for vac distilation.
Add to one litre of acetonitrile, 3moles (367.65 grams) of potassium carbonate and then add ten grams of tbab (tetrabutylammoniumbromide). Stir this mix with mag. stirrer/hotplate at 50 to 60 deg cel. for 15-20 minutes. Next add 1 mole (135.5 grams) of 4-piperidone mono hydrochloride in very small amounts so as the c02 evolution is not too vigorous. ie. ADD TINY AMOUNTS OR THE CHEMICAL REACTION WILL CAUSE THE SOLUTION/REACTION TO "JUMP" RIGHT OUT OF YOUR FLASK. After the complete addition of the 4-piperidone is finished, stir at 50-60deg cel. for an hour. Now place your reflux condensor in the middle neck position and add a stopper to one of the angled necks that are left. Start the water thru the condensor and make sure the stopper and condenser are secured snugg and tight, with adequate amounts of "silicon-vaccuum-grease", so as to ensure a tight seal. This will leave "one" neck open.
Now take your sep. funnel/addition funnel and connect to the last open flask neck making sure the funnel is in the "closed position". Add 1 mole (185.06 grams) of phenethyl bromide to the funnel bearing in mind that you need to turn on the funnel so as to "drip" the chemical into the flask very very very slowly. Once the full amount of phenethyl bromide is added, turn off the funnel and turn on the mag. hotplate-stirrer/oil bath to a mild "reflux" temp.....just get it "simmering"...at around 110 to 120 deg cel. This will facilitate a mild reflux...continue for 24 hours.
As this chemical mix reacts, after a few hours of reflux, you will notice a change from a "clear" solution to a more distinct reddish-brown color. The potassium carbonate will not dissolve into the solution as it will continue to stay in its powder/granual like state during the whole synthesis. It is there to absorb the by product of the reaction, so it does not need to dissolve.
After the 24hr reflux, cool the solution to room temp and filter out the potassium carbonate.(it will look like a white yellow powder at this point) You can throw this out, as you only want to save the "reddish-brown" liquid. Take this liquid/solution and put it back into your three neck flask......cap off one side and middle neck with stoppers, attach distillation condensor vaccuum adapter-receiver flask, and turn on water cooled condenser jacket. Turn on vaccuum pump and heat at 100 deg cel. You need to evaporate as much "solvent" out of the solution as possible with out **BURNING-IT**...So use as little heat as possible and once the solvent starts to "come-over" into the receiving flask, maintain the lowest temp so as to facilitate flow, until
a thick sludge/tar forms on the bottom of the flask. It will be a very dark reddish-brown in color and very very sticky and tar like. (you can use the mag stiirrer in this process...in fact I would recommend you do to keep it from burning).... When you get a thick tar and have finished
distilling off the solvents (discard solvents properly or save), dissasemble distillation setup, add 500ml acetone to the rb flask with the tar and swirl until dissolved. Crystalization will occur and you can filter off the n-phenethyl-4-piperidone crystals or use a more familar
"solvent" of your choice that is compatible with the synthesis. Once the n-phenethyl-4-piperidone crystals are filtered out of the solvent spread them on a small pyrexx baking pan or similar to enable evaporation. To speed up this process, you can heat the pan very very mildly.
YOU HAVE TO REMEMBER THAT THE PRODUCT HAS A MELTING POINT OF 68 DEG CEL SO YOU WILL POLYMERIZE AND RUIN YOUR PRODUCT IF YOU HEAT TOO MUCH. So be careful during evaporation!! You should have roughly 120 grams of product **N-PHENETHYL-4-PIPERIDONE**...which is the "main" precursor for
the "FENTANYL" synthesis.
