Making Testosterone from Androstenedione

[Bean]

Please make this a sticky; this is the article typed out from the Dirty Dieting News Letter #2 dated May of 1997
Comments on making this into an injectable are welcome as are inputs on converting other PHs like 1,4-andro.
To the mods: You have my permission to fix my spelling and paragraph appointments (dunno how to do that)



Editor's Note: In the US, this chemical procedure is illegal. Additionally, the by-products of the various androstenediols may fall under the Federal Analogue Act, which schedules derivatives of any DEA-controlled drug (in this case testosterone) into a Control I substance. So in effect, this procedure outlined is a hypothetical exercise designed to show a possible conversion of androstenedione to testosterone.

The procedure outlined below won't convert 100% of androstenedione to testosterone. But it will convert at least 60% of it, if the procedure is not screwed up too badly. the other percentage of finishied product will contain a small amount of unreacted androstenedione and a larger amount of a (epimeric) mixture of 3,17-androstenediols, which, fortunately, are safe and considerably anabolic compounds in their own right.

Materials Needed

1. Androstenedione (powder)
2. Methanol (wood alcohol)
3. Sodium Borohydride (sodium tetrahydroborate)
4. Acetic Acid (ethanoic acid)
5. Distilled Water
6. Litmus Paper
7. Thermometer (Fahrenheit)
8. Also: Beaker or glass container for the reaction a pot for salt water ice bath, a way to stir (i.e. spoon), filter, eyedropped (1 or 2cc size).
   [/list=1]
   
   Procedure
   1. 10 grams of androstenedione is dissolved in 400ml methanol and cooled to 32deg Fahrenheit in a salt/ice bath (similar to chilling home-made ice cream).
      
   2. 2.5g sodium borohydride is added while the solution is stirred.
      
   3. The solution is continually stirred for 45 minutes while the temperature is maintained as close to 32deg Fahrenheit as possible.
      
   4. After 45 minutes, acetic acid is added to the solution, while stirring, in increments of approximately 2ml at a time (hydrogen gas will evolve).
      
      WARNING!
      Hydrogen Gas can ignite from flame or spark.
      
   5. After each addition of acetic acid, thepH of the solution should be checked.
      
   6. When the pH just begins to turn acidic on the litmus paper, then the addition of acetic acid should be stopped.
      
   7. The methanol solution is now concentrated by evaporation until the volume is around 50ml.
      
      WARNING!
      Hydrogen gas may still be present; it can ignite from flame or spark.
      
   8. This concentrated methanol solution is then mixed with 700ml water.
   9. The cloudy precipitate that forms is filtered off and the filter cake is washed extensively (several times) with water.
      
   10. The filter cake can be air (sun) dried for several days or dried in an oven for several hours at a temperature no higher than 150deg Fahrenheit.
       
   11. The finished product, a fine white powder, should contain approximately 60 to 80% testosterone, with lesser amounts of unreacted androstenedione and a mixture of 3-alpha, 17-beta, and 3-beta, 17-beta androstenediols.
       [/list=1]
       
       What should be done with this (now highly illegal) stuff once the procedure is finished?
       
       Since it is highly illegal I would advocate getting rid of it.
       
       Yet if someone wanted to take the risk and decided to use it, they would probably wonder if it should be taken orally or what?
       
       I would not suggest that anyone take it orally because the purpose of the experiment would be defeated. Since testosterone is mostly deactivated in the gut, the ingestion of the finished product would be worthless. Instead, there are better alternatives, such as making sublingual liquid by dissolving the product in a solvent such as propyleneglycol and/or ethanol. If this is done, I suggest aiming for a concentration of around 30mg/ml and taking one-third of a milliliter (about 33 insulin IUs) under the tongue as a single dose (repeated throughout the day as often as wished by the user). Another alternative is to make a transdermal DMSO solution (messy and stinky). A third course of action (for the bold ones) is to make an injectable solution. There is a fine art to making such solutions (oil- and aqueous-based) and it is beyond the scope of this article for me to go into this. Perhaps that will make a future installment if we have a response to do so.

 

[ex_banana-eater]

wow, never thought anyone would write it up. karma for you.

 

[curt2go]

Has anyone ever tried it? Talk to ya

 

[wojo]

what no karma for me im the one that found it..lol

 

[curt2go]

For something that is unproven... hehehehe. Talk to ya..

 

[wojo]

im sure it has been proven..considering how old the procedure is there should be some post somewhere on a board im going to check both qfac and elite and see if i can find something

 

[b-boy]

alright!!

great post bro, i was just reading it yesterday from the newsletter i download a some time ago and it was kinda hard to read and hard on my eyes..lol.. thanks for saving my eyesight bro.

 

[drfly]

hey bean, thanks for taking my advice and typing this up for us all, it was hard to read before and i think this will help a lot of people. hopefully this will become a sticky

 

[pogue]

see this thread for more discussion:

http://www.bdcnutrition.com/forum/showthread.php?s=&threadid=869

 

[pogue]

Question - what are these and where can I get them:

Methanol (wood alcohol)

Sodium Borohydride (sodium tetrahydroborate)

Acetic Acid (ethanoic acid)

 

[wojo]

dont quote me as im an idiot and not affraid to acknowledge it..lol..but methanol is heat and acetic acid is vinegar

 

[weissmuller]

Originally posted by pogue
Question - what are these and where can I get them:

Methanol (wood alcohol)

Sodium Borohydride (sodium tetrahydroborate)

Acetic Acid (ethanoic acid)

Methonol or Wood Alcohol is also known by the name Denatured Alcohol and should be availible at any home improvment store.  Its used as paint thinner, solvent for oil based paints.

Acetic Acid is just your good old vinegar.  Sodium Tetrahyroborate is a chemical is a reducing agent commonly used in chemistry.  There would be no problem in any of us aquiring it through these means seeing as it is very legit and not watched, but that method is gonna be harder and more expensive.  I believe Benn mentioned its use in some chemical cleaner or other product in the other thread.  Maybe he or someone else can shed some more light on that.

The litmus paper can probally be aquired at a pool supply shop but again is another item easily ordered from any chemical supply company. 

The glass where needed could probally be found at Walmart seeing as only a measuing container and assorted glass containers are needed.  Measuring the mL of acid in small quanities can be done with a mL calibrated eyedropper sold at most drug store for use in dosing children medicine(as a side note: also wounderful for measuring out individual doses of transdermals and makes application much easier.).

The hardest part will be measuring the Sodium Tetrahyroborate in such an a small amount.  But if you walk into your local post office when no ones looking, there postal scales might work.  Or you could find a friend dealing in drugs or just visit a school lab.  If someone wished they could use a large excess(1 TBSP should be more than enough) but this could create more hydrogen gas and would require more filtering.

But overall this is pretty simple and very economicly pleasing and might help out some bros who can't find esterless test powder or are woudering what to do with that extra andro-dione they have lying around.

 

[pogue]

Alright, here is what I've found

Sodium borohydride appears to be an agent found in certain soaps and laundry detergents, but I couldn't find an individual place that sold it by itself, except in China. However, from reading it appears to be very dangerous and anyone that does this procedure should wear gloves, goggles and a face mask. Keep away from open flames, and keep the chemicals away from each other. Here is an article on safey when using sodium borohydride:

http://www.jtbaker.com/msds/englishhtml/S3146.htm

Methanol appears to be used in car racing fuels and probably fuel additives. Your local auto parts store might have this, or you might have to look in the phone book and call around to see if you can find some racing fuel. Auto shops, custom shops and places like that will probably carry it, and it might be in some fuel cleaners and octane boosters.

Otherwise, you can get it here -

Sunoco Methanol (99.95%)
Item Price:$ 41.95
Sunoco Methanol: Clear, 5 gallons in an UN/DOT approved container that is reusable. UPS/FedEx HAZMAT fee ($20) INCLUDED for each container. Shipped in a double wall box per UPS requirements. Shipped FedEx or UPS Ground or 3 Day Select. NO AIR SHIPMENT. Taxable in Texas. NO HAZMAT service outside of USA's 48 contiguous states.

http://www.goemerchant7.com/index.cgi?PageToView=catalog&Department=81051&Cartid=&Merchant=highfuelsn&ExpandedDepts=

Obviously, this is very flammable as well and is pure wood alcohol.

Finally, Acetic Acid is found in vinegar, but in 4-8% concentrate. Not sure if this would be pure enough. Otherwise, here is what I found.

"You should be able to get regular 28% acetic acid in any large photo store or chemical supply store...
Look in your yellow pages for photographic and chemical supply. You should be able to drive up and pick this stuff up."

"28-30% acetic acid is available in the US from Oriental grocery stores. I have never seen it in normal stores. "

 

[pogue]

Looks like weissmuller got to it before I did.

Would the amount of acetic acid in vinegar be enough for this experiment?

Sounds like the wood alcohol will be easy to get, but what about the Sodium Tetrahyroborate? It sounds like its hazmat. What is it used for legitimately? We need to find a source for this, it seems to be the most difficult to attain.

As for a small scale, a food scale would work, and the drug dealer scales you are talking about are known as "monkey scales" and can be purchased at your local head shop. They're a couple bucks. Most zip lock baggies weigh 1-2 grams btw. Also if you know someone who has one of those home stamp weighers or things like that, it would also work. Anyways, thats a side note.

The main thing is getting all the chemicals.

 

[weissmuller]

Well the sodium tetrahydroborate is gonna be a little bit of a pain.  Springfield Scientific does carry it and will most likely ship it out, the downside is you have to purchase 100 g and with hazmat fees and special packaging its gonna run close to $100.  Plus Springfield has is in the process of moving and that might mean its not shippable and would cause a long wait.

A havn't gone searching for other sources in commercial products but I'll look into in the morning.  If anyone wants to post some info to jump start my search(anything its conatined in) it would be appericiated.

Acetic acid concentration isn't a big deal.  Its only purpose is a hyrdronium inon source to complete reduction.  The lower the concentration the more you'll need.  Not a big deal though cause with standard vinegar using the above procedure rough calculations(very rough) make me believe around 42 mL would be needed.  But don't trust the number.

Also those saftey reports are really overdone.  Sodium tetrahydroborate shouldn't be much more dangerous than a strong acid (not to say thats safe), but I wouldn't expect anyone to die from minimal exposure.  But saftey is the center of any experiment and all precautions should be taken.  Definately eye protection, hand covering, and clothing that dosn't leave any exposed skin.

 

[b-boy]

well

i got the acetic acid and methanol covered.. i work at a chemical plant and we have large totes of pure acetic acid and methanol in large drums,,,, working on the other ingrediants... may have to ask one of the chemical engineers when they get back from the holidays 

 

[pogue]

Re: well

i got the acetic acid and methanol covered.. i work at a chemical plant and we have large totes of pure acetic acid and methanol in large drums,,,, working on the other ingrediants... may have to ask one of the chemical engineers when they get back from the holidays 

excellent, if you wanted to sell some (looks like we need just a little bit of everything) i would be interested!

you could start selling andro conversion kits to everyone

 

[Bean]

hey no prob guys. just tryin to do my part

conversion kits sound kickass reminds me of fina kits, lol

 

[b-boy]

Re: Re: well

Originally posted by pogue


excellent, if you wanted to sell some (looks like we need just a little bit of everything) i would be interested!

you could start selling andro conversion kits to everyone

sell? naw free for all my good bro's at bdc, I don't sell nothing bro.

 

[ex_banana-eater]

why not just buy some test base from overseas?

 

[lovetoeat]

Anyone know where to get andro powder, it should be cheap as hell.

 

[pogue]

why not just buy some test base from overseas?

easier said than done, don't know where to get any - besides, this is an interesting discussion of how to convert a legal substance into an illegal one

Anyone know where to get andro powder, it should be cheap as hell.

http://www.myvitanet.com/an30grambul.html

There has been discussion that the PHs from that site are not very good, but its the only place I've seen that still sells andro powder.

 

[b-boy]

ha

Originally posted by ex_banana-eater
why not just buy some test base from overseas?

considering all my ingredients are free and the price of andro...LOL  its cheaper for me to make it...

 

[wojo]

yeah this sounds way too much like a hassle plus its easy as hell to find a source

 

[weissmuller]

Sodium Borohydride(Source)

Okay I did some hunting around and found a source of Sodium Borohydride in the quanities we need.  They sell it in either 5 or 10 g packs.  It'll still cost about 30 shipped for 10 g, but thats better than the alternative sources I've been checking out.  This source also works with individual and shouldn't have any problems.

I've never worked with this site so it dosn't have my guarantee but if I am ordering some this is where I am getting it from.

http://www.postapplescientific.com/reagents/sa-sh.html

 

[Bean]

yo mods, can we make this a sticky?

 

[SteveDFW]

I posted this in the "Making testerone from Adro..." threat but here it is again:

BAC has andro powder at 20 grams for $14

http://www.beyond-a-century.com/

 

[pogue]

bump

anyone gonna try this?

 

[Lifeguard]

I noticed that you said the conversion is for androsteneDIONE...

you can use androsteneDIOL right??

and what about the other androgens....such as....hmmm...1,4-andro, 19-Nor-4-andro, 5-AA??

Would the conversion work for those ones too??

 

Cuz, quite frankly, that would kick royal ass

 

LG.

 

 

[drfly]

no, LG, currently we only have the procedure developed for converting DIONEs to their target hormones, but i believe we have some people working on getting a formulation for converting diols. as for the other ph's, yes, theoretically they should all work so long as they r diones, eg. 1,4-dione, 19-nordione, and the like.

 

[Lifeguard]

Originally posted by drfly
theoretically they should all work so long as they r diones, eg. 1,4-dione, 19-nordione, and the like.

Works for me

 

LG.

 

[candle25]

I know this is an old thread, but has anyone tried this. I would be glad to but I don't have access to HPLC. I have friends at another lab that can run it for me though.

 

[mass_builder]

bump for the idea

 

[Milo Hobgoblin]

Bad News....


During my stint in Molecular Bio I studied steroid chemistry for two years.

This experiment is EXTREMELY hard to do even with the appropriate lab materials and here is why. (I acutally did this expeirment BTW... but I started even further back.. FROM CHOLESTEROL LOL)

The melting points of many of the intermnediates is extremely low... which means that many of the steps have to be performed under low pressure conditions to get a boiling point well below the temop. at which the compnmenets just turn to goo (Im trying to use laymans terms here... sorry)

I used a mercury vacuum and ice-salt baths and my eventual yield was EXTREMELY low...

PLUS

many of the components some of you are talking about have to be COMPLETELY dry (i.e stored in sodium... very dangerous and VERY hard to get)

ANY water at all at ANY point in this experiment will completely destroy ALL your work.

TRUST me... this is a PAIN IN THE ASS.

If you want EASY homemade test without having to give yourself a stroke.. just do the extraction from the vet pellets 9synovex)... its much easier and you'll get a high yield... you can be sloppy and it still works.

LOL Im laughing to myself remembering what a pain in the ass it was to keep that fucking methanol dry.

OH YES!!! one more thing

What the author FAILS to tell you!! is that you WILL have a considerable concentration of dihydrotest...

It would be very difficult to selectively reduce the 17 ketone group and NOT the 3 ketone group.

as a matter of fact you would have strange mixtures of all kinds of weird analogues from uncontrolled reductions and oxidations during various steps.

Oh... just to let you know... I had access to IR and an MR to determine purity... and of course high quality equipment to measue melting points.

It was a REALLY fun experiment though... I would rather inject toilet water (jk )but seeeing that powdewr in the end was a total thrill.

 

[candle25]

Well bro I've already ordered the Andro and I get the other chems free. I'm going to try it anyhow and see how it goes. I have access to IR & HPLC so I'll be able to test purity easily. I think your problem must have come from starting with cholesterol. I've seen the method for that and have no intrest in it...lol. I know there will be some radiance structures formed as byproducts, but they should be safe IMO. As for keeping chems dry, NaBH4 shouldn't be a problem, and Methanol doesn't seem like it would be difficult either. I agree about the syno conversion. This is just cheaper...if it works. I'll keep everyone posted on this thread as to how my experiment goes. It will take some time so just hold tight...

 

[Milo Hobgoblin]

cool. good luck.

make sure that sodium borohydride is super clean and sealed... if even a small amount of moisture got into the bottle (even from humidity) it will kill the reaction.

I used a similar compund (I cant remember exactly but it was an aluminum based catalyst) and the lid wasnt sealed properly... thanks to the humidity.. it ruined the compound and about 10 hours worth of work.

Make sure you have a good vacuum too.. I ended up breaking ours and sucked mercury through it LOL.

and yes starting from cholesterol increased the difficulty ten fold.

I still cant see how this reaction is going to selectively reduce that group. I would think you would have to protect the C-3 group and reduce c-17??? but I dont see a mechanism for doing that in the initial reaction??

Its been a LONG time so maybe Im just missing something.

 

[candle25]

A bro at SM suggested this:

It can actually be a bit better than that. By doing the reduction in 30% methanol in dichloromethane at -78 deg C, a 93:7 mixture of testosterone to 3b,17b-diol can be obtained.

Reference: Canadian Journal of Chemistry, (1989), 67, 1206-1211.

I'll most likely try this if I can get some dry ice to get the temp low enough. As for the vacume, do you mean atmospheric pressure or just a filtration vacume? I plan on doing this reaction at atmospheric presssure, IOW in an open beaker.

 

[sicosico]

someone eles should try doing this post :

JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
#75 (1953)
page 5930
sondheimer et al.

1g 4AD + 100mL chloroform + 10g MnO2 = test base 100% after 2 hours shaking at room temp

yield is 93% when crystalized with methanol and filtered on paper

MATERIALS: (check www.sciencelab.com i don't know if they are the cheapest, but they have everything)
beakers
hotplate with built in stirrer
stirring bars
distilled water
methanol
chloroform (can be cheaper grade)
thermometer (-10 to 150 degrees celcius, its like $4)
4AD powder
activated MnO2 (if this cannot be found, make your own from potassium permanganate and manganese sulfate. also need ether if you do this step)
filter paper
funnel (holds filter paper)
earlmeyer flask with vacuum tube out side for vacuum filtering
scale

now that is alot of MnO2 and it can be done with less. too simple you say, well your right its not that easy. the MnO2 available commercially is not always active. but the authors gave a method of preparing MnO2 that is easy and the product is very active and can be put in a stoppered jar with no loss of activity (those guys would make great homebrewers)

HOW TO MAKE MnO2:

take concentrated aqueous potassium permanganate and add to a stirred aqueous manganese sulfate solution kept at 90 degrees celcius (need a hot plate that has stirrer built in) until a slight excess was present (pink coloration of the supernatant liquid). stir at 90 degrees celcius for 15 minutes. filter, wash well with hot water, then methanol and ether. dry at 120 to 130 degrees celcius to a constant weight. it can be kept for several months in a well stoppered bottle with no loss of activity.

how to get concentrated aqueous potassium permanganate: take distilled water and and add potassium permanganate until not more goes into solution (this is where a magnetic stirrer comes in handy). if you added too much, just add more water until all is in solution. duh!

how to get aqueous manganese sulfate: same idea as above.

METHOD:

i am looking for a source of activated manganes dioxide so that the above does not need to be performed. once we get the manganes dioxide, all we have to do is mix the 4AD, MnO2 and chloroform in the ratios above, basically add the 4AD to chloroform on the magnetic stirrer and then add the MnO2 and leave it for 3 hours at room temp. add methanol to the solution and the test will crystalize and fall out of solution. filter and wash well with methanol. collect the filtrate and filter again on new filter paper and dry all the filter papers. if the filtrate still has crystals, filter with another paper. i would dry the first filter paper out well for a few days and weigh it. if its more than 80% yield, i wouldn't waste time trying to get the rest. if not, then take the filtrate and refilter to get rest of crystals. you kind of play it by ear. that's pretty much it.....oh yeah, don't forget to discard the powder properly as this is an experiment

it is possible that much less MnO2 can be used. this will mean that the reaction will have to sit longer maybe a day or two, i don't really know. this will have to be found out. i want to try this in the lab where i can measure the ultraviolet spectrum to determine how long the complete reaction takes with different amounts of MnO2 and chloroform so as to minimize cost.

 

[sicosico]

or try doing this : from superior muscle:

BOLDENONE CYPIONATE (fast acting EQ)

Step 1: 1-Test cyp is brominated in the 4 position with 2,4,4,6-tetrabromocyclohexa-2,5-dione in ether with catalytic HCl. The product is 4-bromo-1-testosterone cypionate. There are other methods to achieve this bromination as well but this one should work very cleanly with a minimum of side reactions.

Step 2: the bromide is eliminated to give the 4,5-double bond by stirring the above product in DBU for 10 to 20 minutes. The overall yield of bold cyp should be around 75 to 80%

METHANDROSTENOLONE (dbol)

Step 1: The bold cyp from above is stirred in boiling benzene with ethylene glycol and catalytic acid. A Dean-Stark trap should be used to remove water as it is formed. This protects the 3-one as an ethylene ketal.

Step 2: The above protected bold cyp is stirred in boiling methanol/water with NaOH to remove the cyp ester.

Step 3: The 17-OH is oxidized to a ketone with any of a variety of chromium VI reagents.

Step 4: The above 17-one is reacted with methyl magnesium iodide. The reaction is quenched with water and acid. Heating the mixture with the water and acid will remove the ethylene ketal as well, leaving you with methandrostenolone.

METHENOLONE CYPIONATE (Primobolin, although real primo is the enanthate, not the cypionate, I expect little difference in function.

Step 1: 1-Test cyp is reacted with tetramethyl dilithium pentacuprate (formed in-situ from CuI and meLi). The reaction is quenched with liquid bromine. The product is 2-bromo-1-methyl-DHT.

Step 2: The bromine is eliminated to give back the 1,2-double bond by stirring with DBU as in the synthesis of bold cyp. The product is methenolone cypionate.

MESTEROLONE (proviron)

1-Test base is reacted with tetramethyl dilithium pentacuprate (formed in-situ from CuI and meLi). The reaction is quenched with water to afford mesterolone in a single step.

OXANDROLONE (Anavar)

Step 1: Starting with 1-test base, the 3-one is protected as the ethylene ketal as in the above synthesis of methandrostenolone.

Step 2: The 17-OH is oxidized to a 17-one with chomium VI reagent.

step 3: The 17-methyl is attached with methyl magnesium iodide and the crude reaction mixture is treated with water and acid to quench the reaction and remove the ketal protecting group. The product is 17-methyl-1-test.

Step 4: the 17-methy-1-test is treated with ozone in methanol and then NaOH is added. This allows the purification of the intermediate by recrystallization of the sodium salt. The result is that the double bond is cleaved to give a carboxyolic acid (salt) on one side and an aldehyde on the other. The salt is dissolved in water and acidified to pH=4. NaBH4 is added to reduce the intermediate aldehyde. The resulting alcohol will spontaniously close with the carboxylic acid to give the desired lactone ring. The product is oxandrolone.

OXYMETHYLONE (Anadrol)

17-methyl-1-test from above is reduced with lithium in liquid ammonia. The ammonia is carefully evaporated under a dry N2 atmosphere to give a dry, crystalline enolate. The enolate is dissolved in dry THF and treated with N-formylmorpholine to give oxymethylone as the product.

DROMOSTANOLONE propionate (Masterone)

Step 1: 1-test base is reduced with lithium in liquid ammonia. The ammonia is carefully evaporated under a dry N2 atmosphere to give a dry, crystalline enolate. The enolate is dissolved in dry THF and treated with methyl iodide to install the 2-methyl group.

Step 2: the dromostanolone resulting from step 1 is esterified with propanoyl chloride and pyridine to afford the product, masterone.

 

[sicosico]

or try this with ando only :

careful reduction of the androstendione with NaBH4 at low temperature will selectively reduce the 17-one to give you test directly without having to reduce everything and re-oxidize the 3-OH.

 

[Milo Hobgoblin]

...

doing ALL these reactions in reduced atmosphereic pressure in closed enviroments will greatly increase yields. Some of them have to be done at lower pressures though. the boiling point of some of the compounds is too high at standard atmospheric pressure and will just turn to a sticky yellow goo that yields nothing.

You will have to redo the calculations for lower boiling points and catalyst reductions.



LOL superior muscle makes it look so easy.

 

[candle25]

Spidey from SM is a Phd in chemistry. He and I have been talking about some of the reactions that sicosico posted. Most are of interest to me, but one thing at a time. I have access to a large variety of chems for free, but not everything. Anyone who has ordered from fisher or such knows that chems are pricy. Sometimes shipping on hazardous chems are more than the chems! I would like to try most conversions, but only if it is at a minimal cost to me. Thanks for the info Milo. I'm still going to try this at atmospheric pressure as I want to see how things would go for the bro's who don't have access to a lab. I want to keep it as simple a possible.

 

[sicosico]

or try this with ando only :

careful reduction of the androstendione with NaBH4 at low temperature will selectively reduce the 17-one to give you test directly without having to reduce everything and re-oxidize the 3-OH.

this seams the easiest conversion ! only one step

 

[candle25]

You might have noticed that this thread is about that exact conversion. I'm working on it...lol

 

[candle25]

I finaly have all the chems together to do this. I'll pick up the dry ice tommorrow and get started. The only problem now is that all the labs I know and have done buisnes with don't test things like Testosterone. So now I'm stuck looking for a lab that will test it for me. So far the few I've called were not suspicious. Anyone have a lab in mind? Also, I'm concerned with having to ship it to a lab. Does anyone think I might have a problem with doing that?

 

[candle25]

I'm in the middle of the conversion right now. I still haven't found a lab to test the product for me so I might have to go by MP. Here is the reaction scheme for anyone interested:

 

[candle25]

My first attempt at this went aweful. I spilled lots of the crude product during the filtration process. Gravity filtration of this is impossible so I ended up using a vacume filter. My kitchen stank of evaporated MeOH & the acetic fumes burned my eyes. This isn't something to attempt without the proper equipment! My yield in the end was only around 2.5g of a white, epoxy type material. For MP testing I used Ethylene Glycol since its BP is 199C and pure Test's MP is 155C. The melting range of my product was 125C-127C which means that I didn't make TNE at all .

I still have 50g of Andro & all the chems I need to do the experiment again so I might do that soon. I might use a dry ice/acetone bath to cool the reaction to -72C next time to see if it makes a difference. I suspect that the place of error was in the evaporation of MeOH. Even at a rolling boil it was very hesitant to evaporate? Anyhow, I'm going to discuss this with Spidey from SM & see what we can come up with. I'm not giving up yet...lol

 

[PC1]

I admire your knowledge and determination. A great thread to read, best of luck with it

 

[x_muscle]

My first attempt at this went aweful. I spilled lots of the crude product during the filtration process. Gravity filtration of this is impossible so I ended up using a vacume filter. My kitchen stank of evaporated MeOH & the acetic fumes burned my eyes. This isn't something to attempt without the proper equipment! My yield in the end was only around 2.5g of a white, epoxy type material. For MP testing I used Ethylene Glycol since its BP is 199C and pure Test's MP is 155C. The melting range of my product was 125C-127C which means that I didn't make TNE at all .

I still have 50g of Andro & all the chems I need to do the experiment again so I might do that soon. I might use a dry ice/acetone bath to cool the reaction to -72C next time to see if it makes a difference. I suspect that the place of error was in the evaporation of MeOH. Even at a rolling boil it was very hesitant to evaporate? Anyhow, I'm going to discuss this with Spidey from SM & see what we can come up with. I'm not giving up yet...lol

maybe you should centrifuge for filtration. how did vacuum filter in your kitchen?.......do u have buchner funnel and a vacuum?......if you have these equipments why did you boil the solution to get MeOH you can simply use vacuum filtration in a flask, then spread the powder in a watch glass and it will dry in 10 min, then you can wash the residue with water.

are you using recrystallization to get impurities out?
and maybe it sounds funny but wear goggles next time

 

[candle25]

I took the solution to work and filtered it. I'm a chem E at a pretty nicely equiped lab. The procedures were to condense the MeOH/Test solution and then crystallize by the addition of water. The original abstract that this idea was taken from did so as well. It might not crystallize otherwise as the solution wouldn't be as saturated. Are you suggesting that I attempt to crystallize without condensing?

BTW, goggles don't help much with fumes....lol