Making Testosterone from Androstenedione
12-24-2002 05:16 PM
Anyone know where to get andro powder, it should be cheap as hell.
12-24-2002 05:38 PM
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 Originally posted by ex_banana-eater why not just buy some test base from overseas?
http://www.myvitanet.com/an30grambul.html Originally posted by lovetoeat Anyone know where to get andro powder, it should be cheap as hell.
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.
12-24-2002 08:02 PM
considering all my ingredients are free and the price of andro...LOL its cheaper for me to make it... Originally posted by ex_banana-eater why not just buy some test base from overseas?
12-24-2002 08:25 PM
yeah this sounds way too much like a hassle plus its easy as hell to find a source
12-24-2002 09:13 PM
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.
12-27-2002 01:25 AM
yo mods, can we make this a sticky?
12-27-2002 12:07 PM
I posted this in the "Making testerone from Adro..." threat but here it is again:
BAC has andro powder at 20 grams for $14
01-03-2003 07:12 PM
anyone gonna try this?
01-04-2003 07:47 PM
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
01-04-2003 09:20 PM
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.
01-04-2003 10:32 PM
01-03-2004 03:23 PM
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.
01-04-2004 03:23 AM
01-05-2004 10:37 AM
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...
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 ****ing 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.
01-05-2004 11:54 AM
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...
01-05-2004 02:59 PM
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.
01-05-2004 03:11 PM
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.
01-05-2004 04:29 PM
someone eles should try doing this post :
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
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)
hotplate with built in stirrer
chloroform (can be cheaper grade)
thermometer (-10 to 150 degrees celcius, its like $4)
activated MnO2 (if this cannot be found, make your own from potassium permanganate and manganese sulfate. also need ether if you do this step)
funnel (holds filter paper)
earlmeyer flask with vacuum tube out side for vacuum filtering
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.
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.
01-05-2004 04:30 PM
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%
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.
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.
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.
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.
01-05-2004 04:30 PM
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.
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