Saponificaion of tren acetate ester for transdermal prep *EXPERIMENT*

Chemo

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General steps are:

  • Dissolve in MeOH (methanol, methyl alcohol, wood alcohol, HEET).
  • Add NaOH to cleave the ester.
  • Wash with water and neutralize.
  • Dry, weigh, and dispose.
Reference the attached spreadsheet for yield calculation, reaction scheme, and procedure.

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Billy_Bathgate

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Acetone work out as well?

Thats what I have always leaned towards...not a methanol fan really :)
 
Chemo

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Originally posted by Billy_Bathgate
Acetone work out as well?

Thats what I have always leaned towards...not a methanol fan really :)
Acetone works as does MEK and any other polar carbonyl solvent.

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Billy_Bathgate

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That is what I presumed...but you have suprised me with a couple curve balls lately so thought Id better ask!
 
pogue

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Seems simple enough. Can this process also be used to remove the estradiol from synovex? The procedure looks the same.
 
Chemo

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Originally posted by pogue
Seems simple enough. Can this process also be used to remove the estradiol from synovex? The procedure looks the same.
It does work but you will need much more NaOH so neutralize the estradiol and make it a water soluble salt.  In other words, it will work but for different reasons.  I plan on writing a summary of the techniques for producing BOTH TNE and TP from syno with no kit needed sometime in the near future.

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The Answer

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This does seem like a very interesting experiment. And actually it seems "do-able"

Thanks
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Billy_Bathgate

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Top of your head chemo...

Youd need at least a 1:1 to remove the ester...to be safe maybe a 2:1 even (OH:Hormone)

Whats it for estrogen soluability...I was thinking maybe 5:1
 
Chemo

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Originally posted by Billy_Bathgate
Top of your head chemo...

Youd need at least a 1:1 to remove the ester...to be safe maybe a 2:1 even (OH:Hormone)

Whats it for estrogen soluability...I was thinking maybe 5:1
Actually, to saponify the ester it does not even require a 1:1 molar ratio since the -OH is used a CATALYST.  Obviously, if you use more than necessary it will just speed the rate of the reaction.

As for the estrogen solubility...I reserve the answer to that for the mini-article I'm about to post about the making TNE and TP from syno.  In a nutshell though, a 10:1 will ensure proper salting of estradiol and choice of either a small, strong base or large, hindered, strong base will determine product (esterfied or not).

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Billy_Bathgate

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1:1..hmm. I was thinking that the OH- substituted the ester. Thats where I came up with that, but actually, I now think from your reply that H+ is reacting with the ester, and that is what "cleaves" it?

The OH just probides the basic solution?

You got me on the edge of my chair thinking. Ive even busted out my chem book a couple times :)
 

Matthew D

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Correct . It is lye one of the commerical brands is Red Devil Lye at least here in the states.
 

syko

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Attaway to come through. So just plain lye? Wow i am having a Tyler Durden flash back. Sweet that makes it so much easier. Will their be pictures posted to go along with the procedure? Wink Wink Cough cough.

thanks peace.
 

syko

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One more ? pls. The tren acetate is this after a finakit conversion?

thanks peace.
 
pogue

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Attaway to come through. So just plain lye? Wow i am having a Tyler Durden flash back. Sweet that makes it so much easier. Will their be pictures posted to go along with the procedure? Wink Wink Cough cough.

thanks peace.
I'm going into my cave, I'm going to find my power animal...
 
pogue

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One more ? pls. The tren acetate is this after a finakit conversion?

thanks peace.
This experiement is for removing the acetate ester to use fina via transdermal application. The fina pellets already have the ester attatched, so by removing the ester, you get a higher absorption. If you are using the kit, you don't need this procedure.
 

syko

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I must be missing something here then what about the estradiol? Is that removed on the saponification process?
Or is it not absorbed vea trans?

Sorry just getting it all down thanks though.

peace.
 
pogue

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I must be missing something here then what about the estradiol? Is that removed on the saponification process?
Or is it not absorbed vea trans?

Sorry just getting it all down thanks though.

peace.
There is no estradiol present in Finaplix-H or Component-TH. There is estradiol in Synovex-H and some other fina and syno compounds, but regular fina is just tren acetate.
 

syko

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RRRRRRRRRRRRiiiiiiiiiiggggggggggghhhhttttt thanks, sorry for the ignorance, just learning.

pictures?

peace.
 

syko

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Would this work for test prop powder also?

thanks peace.
 

syko

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OIC thanks, again.

lol, has chemo posted the mini-article yet?

peace.
 
wojo

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ok i too came in a little late to this..but wouldnt daze's procedure from mind and muscle mag work here after all it is removing a ester
 

syko

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B I N G O !!!!!!!!!!!!!!!!!!!!!!!!!!!1

ok i too came in a little late to this..but wouldnt daze's procedure from mind and muscle mag work here after all it is removing a ester
I knew i had a procedure to do that somewhere!!!!!! Score :D !!!!!!!

Thankyou very much .

you get karma and so do you pogue for being so patient.

peace.
 
wojo

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The Synovex Solution
by Dazed


Cattle implants are an easy way for the average guy to get his hands on some of the good stuff. Trenbolone acetate is the most popular of this form of steroid as it easily separated from Finaplix or Component pellets. It is usually made into an injectable or topical doseage form. Synovex-H is a lesser known implant that contains 2 grams of testosterone propionate (TP) and, unfortunately, 200mg of estradiol benzoate (EB) per cartridge. Synovex is even more readily available than Fina, and can be found with a simple internet search. No proof of cattle ownership is usually needed, and 20g of testosterone propionate can be had for as little as $70.

There are several ways to remove the estradiol that are commonly known. One involves using diethyl ether and a freezer, and another involves removing the esters before separating. The former method does not completely remove the estradiol, and the latter is bad because the pharmokinetics of straight testosterone in oil are less than desirable (the free base is better for transdermal preparations, however, and will be covered later). Ideally, we could remove the esterified testosterone, without the estrogen.

Good news! I’m going to explain, step by step, how to separate pure testosterone propionate from the estradiol benzoate. The technique is basically a recrystallization of a supersaturated solution, which is commonly used in chemistry to purify substances. I will go through the method with the approximate amounts of chemicals needed to do one cart of Synovex-H. One cart refers to one green cartridge, which is a green cylinder full of pellets, and all together contains 2 grams of TP and 200mg of EB. The actual amounts of chemicals will vary every time you do the procedure, because variables such as temperature and atmospheric pressure are never the same all the time.



Recrystallization


Materials needed: Methanol (Heet) -- The amount needed will vary with the number of recrystallizations. Distilled water, 2 glass containers (Jars preferably), a 60ml syringe, syringe prefilter (.8 to 1.2 micron) and coffee filters.


Note: Be sure to get regular Heet in the yellow bottle. Read the label and use it if it contains ONLY methyl alcohol, and only methyl alcohol.



The Theory (a.k.a how the hell does this work?)


In this method, we take advantage of the fact that there is ten times more testosterone propionate than estradiol benzoate in the cartridge. Both TP and EB are freely soluble in methanol and almost completely insoluble in water. As detailed in Weissberger's "Technique of Organic Chemistry Volume III, Part I Separation and Purification." (1), by slowly adding distilled water to the methanol/steroid solution, we can create a supersaturated solution. This supersaturated solution will crystallize; giving highly pure crystals of the substance that was supersaturated in the solution. Since there is ten times more TP than EB, the solution becomes saturated with TP first, so it will crystallize first. The crystals that form will be pure, but all of the TP will not come out of solution when the first crystals form. Only enough TP will crystallize so that the remaining TP in solution will not be extremely supersaturated. For example, if 200mg TP crystallizes, 1800mg will still be in solution per cart. The one thing to be aware of is that after a certain amount of water is added, the EB will become supersaturated and crystallize as well. The only way to know for sure if there is estrogen in your crystals will be to do take a melting point of some of the crystals.



The Nitty Gritty


Dissolve the cart in 80mls of methanol. This will take about an hour. I put everything in a jar and shake it up. Also, crushing the pellets after about 15 minutes of soaking speeds up the process. Let the filler settle on the bottom of the jar. Use a 60ml syringe to draw up the liquid above the filler that has settled on the bottom. You can leave most of the filler at the bottom, as it is a mess to filter.

Put the syringe filter on and filter the solution into a new, clean, dry jar. The solution should be clear. Now we begin adding the distilled water. The water should be added slowly, and when opalescence is seen in the solution, the water should stop being added, because crystallization is occurring. The whole solution needs to be cloudy before crystallization will really occur, do not confuse this with the cloudiness that happens right where the water hits the methanol. Once the solution is cloudy, screw the cap on the jar and let it sit for at least a half hour. The amount of water that you need to add to get crystals is about 13-25 ml. Be sure to add the water slowly after 10 ml or so. Be patient, because the slower that the crystals form, the more pure they are.

Once the crystals have formed, you want to harvest them. Place a coffee filter in the mouth of another clean, dry jar, so that the crystals can be filtered. Swirl the solutions before you pour it to make sure you get all the crystals. Squeeze the excess liquid through the filter. Once the solution is completely through the filter, remove the filter, label it as the 1st crop, and set it aside. This process is then repeated. Water is added to the solution we just filtered until it is cloudy. Seal the jar and let it crystallize, and harvest the crystals. Be sure to label each crop of crystals -- the number of crops needed will vary.

Once all the crystals are harvested, and allowed to dry overnight, it is time to process them. A melting point will be needed for each crop of crystals. The melting point of TP is 120-122 C (248-251.6 F). If estrogen is present, the melting point of the crystals will be lower than this. Our goal is to get the melting point to 120 C (248 F). Most likely all of the first crops of crystals will have some estrogen in them. This is where the procedure gets a little complicated, but if you can do this, you will be successful. To get really pure crystals, just enough methanol is added to each crop of crystals so that all the crystals are dissolved. Water is added drop wise to these solutions until crystals form, just as we did previously. The crystals are harvested, and melting points are taken. It usually only takes a few simple recrystallizations to get a really pure product. The yield will vary each time you try this, but I recommend just doing one cart at a time, until you get the hang of it.

There are many ways to measure melting point, but an easy way to do it at home is to put some about oil in a pan on a stovetop burner. You will need an accurate thermometer, a test tube, and a few milligrams of your crystals. Be sure you can easily tell the difference between 115 C (239 F) and 120 C (248 F) degrees, this small difference is important! Turn on the burner and heat it to about 100 C (212 F). Make sure the temp is stable. Now put the crystals in the test tube and hold this in the oil, but do not let the test tube touch the bottom of the pan. Slowly increase the heat until the crystals melt, and note the temperature. When the crystals melt at 118 C - 120 C (244.4 F - 248 F), you have pure testosterone propionate.



Making an injectable


If you decide you would like to make the testosterone propionate into an injectable form, Here is how to do it at 100mg/ml. Put the crystals in an empty, clean, dry vial. Add 1 ml of benzyl alcohol (USP grade) per gram of TP. Add 8 ml of vegetable oil per gram of TP. Mix this up by swirling it around. Place it in an oven set at about 170 C (338 F) for five to ten minutes to really heat up the oil. This will make it easy to filter. Once it is hot, draw everything up into a 60ml syringe. Put a .45 or .22 micron filter on the syringe, and a sterile needle, and filter the oil into a sterile vial. Be sure to vent the vial with another needle by sticking one needle it the vial, but with nothing on the end, so that the pressure in the vial is equalized. Benzyl alcohol and syringe filters are fairly easy to find on the net. If you ask around one of the more popular discussion boards, someone will probably point you in the right direction. TP is a bit painful, but several people have used this method successfully.



Making a transdermal


If you want to prepare the crystals for transdermal use, you need to remove the ester group. The supplies you need are sodium hydroxide, distilled water, and methanol. Dissolve the testosterone crystals in a minimun amount of methanol. In a separate container, dissolve 1/8 teaspoon of sodium hydroxide in 8 oz of hot distilled water. Once dissolved, add the sodium hydroxide solution to the methanol/test solution. This will turn white instantly. Let this react for a few minutes. Next add an additional 8 oz of water, to make sure all the salt that was formed is dissolved. The white stuff you see is pure unesterfied testosterone, and it should be filtered out. You should run water over the testosterone while it is on the filter to make sure all of the salts and hydroxides are removed. Ideally you would test the pH of the test to make sure all of the hydroxides are rinsed off. Dry the powder and add it to your favorite topical mix.


Editors Note: It would mix particularly well with ONE, not only because of the superior transdermal formula, but because of the synergism of the 1-testosterone with the added estrogen from aromatization of the testosterone.
 
Chemo

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This method presented by Dazed is not recommended as there are more efficient ways to separate the EB and TP. The first few crops from the method above will yield pure TP but you will recover no more than 30-40% before the EB also starts to precipitate.

An easier method for separation would be to use a big, strong, base and salt the EB. This basically means to add something like tert-butoxide (big, strong, sterically hindered base) in a 10:1 molar ratio and allowing the solution to sit overnight. What it does is salt the EB thereby making it water soluble so when one uses water to wash the dissolved powders the EB goes with the water leaving pure TP on the filter paper.

Chemo
 
wojo

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is there anything chemically comparable to tert-butoxide thatwe can buy..or is it available tto us

would this work for removing the acetate ester from tren?
 
Chemo

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Originally posted by wojo
is there anything chemically comparable to tert-butoxide thatwe can buy..or is it available tto us

would this work for removing the acetate ester from tren?
Anything that is big, strong, and sterically hindered will selectively salt the estradiol.

This is focused specifically NOT to remove the ester from tren.  That can be accomplished easily by using common sodium hydroxide.

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An easier method for separation would be to use a big, strong, base and salt the EB. This basically means to add something like tert-butoxide (big, strong, sterically hindered base) in a 10:1 molar ratio and allowing the solution to sit overnight. What it does is salt the EB thereby making it water soluble so when one uses water to wash the dissolved powders the EB goes with the water leaving pure TP on the filter paper.

Chemo
What do you get when you mix KOtBu with water?
 

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When I try to open the zip file from Chemo's first post in this thread, it is password protected. Will Chemo either remove the password protection or will some one post a non password protected file.
 

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Bear with me folks - I'm an engineer, and I'm smart, but I'm no chemist, and certainly not on par with the folks who hang around here. The closest I've come is Chemistry 1 and 2 in my undergrad studies. So, if you want me to design a high-speed communication system - that's easy! Chemistry? Not so easy...

So, Chemo, am I correct in the understanding that

1. Using an alkalai to salt-out the estradiol will work for both 17-beta-estradiol and estradiol benzoate as the ester would be saponified before the estradiol is salted.
2. That a side-effect of the process is that the tren ace/test prop would now be tren/test base, the ester having been saponified.
3. What do you think of the following post that I found somewhere (I know not where)...

Revalor does contain estradiol which will cause gyno easily if this product is used as is. There is a way to remove the estradiol from the implant by doing to following: Gather about 2-3 of the pellets together and grind them up with the back of a spoon and make the pellets into as fine of a powder as you can. Then, get 50 ml of diethyl ether (pretty easy to obtain from any chemical supplier) and mix this combination together in a bowl. You then have to let the solution evaporate allowing crystals to form in the bowl. The crystals that form at the top of the bowl contain the estradiol that you are trying to get rid of. You then need to place this solution in the freezer overnight to help aid in most of the estradiol being removed from the testosterone-ether solution. By the next morning, you will pull this solution out of the freezer and the frozen crystallized estradiol will have risen to the top of the bowl (just like bread rising in the oven, he! he!). You then would scrape or scoop the crystals off the top of the solution and get rid of them. The remaining crystal that are left at the bottom of the bowl contain the Revalor that you are trying to get. Then let them air dry for a while to get the majority of the ether off the crystals. You then need to place these crystals in the oven on a low temperature to get rid of any ether that remains for a few hours and you should have left the dry Revalor crystals that you need with a minimum of ether left in them. Make sure you have let them air dry first though. You don't want to blow up the house by putting a bowl of ether in the oven just because you are a little to fucking impatient to get big. Make sure that it is a electric oven as well, you definitely don't want to use a gas oven for this procedure. Revalor-S cartridges contain 70 pellets apiece. You can't eat the cartridges either.

4. Bill Roberts wrote on T-mag about the salted estradiol "carrying away" some of the testosterone (50% yield of "nasty yellow test"). Perhaps this is nonsense as one would need several estradiol salt molecules to accomplish this, and there is much less estradiol than tren/test to begin with, so how would it take the yield down to 50%?

Out of interest, is there a simple way to esterify something like 1-testosterone THP ether? I did see a paper entitled "Highly selective one-pot conversion of THP and MOM ethers to acetates by indium triiodide-catalysed deprotection and subsequent transesteri�cation by ethyl acetate". To my layman's ear, indium triiodide sounds rather exotic, but I am an academic, so I could concievably find some. Do you think this is feasible?

Thanks - I look forward to hearing what you have to say.

BTW, might tert-butoxide be the "magic solution" or the "estrogen solubiser" from the various kits on the market?
 
ryansm

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Chemo doesn't come around as often anymore
.
 
jmh80

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Seriously, what happened to Chemo? He posted here all the time when I joined and even into last summer.


Tracer - It may be best to send him an email or IM him.
 
Sir Foxx

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Seriously, what happened to Chemo? He posted here all the time when I joined and even into last summer.


Tracer - It may be best to send him an email or IM him.
Pheromones. He can't keep the chicks off him:D
 

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I want to try this experiment. However, I am at a loss as to the amount of Heet and the amount of Lye solution to use in the experiement. I plan on experimenting on two carts. Any help would be appreciated.

Thx, Phred
 
jmh80

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Klaus - you are a great addition to the board, your chemistry knowledge is immense. Do you have a chem. degree?

BTW, dioxane is some pretty nasty stuff. I seem to remember this stuff hangs around in the body for (what seemed like) millenia. Doesn't this have a Benzene-like ability to cause cancer?

Be careful with it, regardless.
 

jcam222

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Can anyone add detail to this great old thread? I am looking for a bit more guidance on the amounts of NAOH to add to the methanol solution.
 

jcam222

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Thanks for the answer Klaus. I am unfortunately going to have to admit my complete and utter ignorance as to how to do what you said. If you could put it in laymens terms I would truly apprecaite it. I am sure there might even be a couple more people out there who would benefit.

Once I have the tren disolved in the methanol I could use simplified step by step. If you have the time its appreciated.
 

jcam222

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Awesome instruction Klauss thanks a million. I sent some karma your way.

Klaus I have read about freezing the distilled water, poking a small hole in container and the putting on ring stand above the solution. It allows a slow drip of water added as it thaws. What do you think of that?>
 

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