Making Testosterone from Androstenedione

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    Milo Hobgoblin's Avatar
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    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.

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    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.
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    Quote Originally Posted by 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
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    You might have noticed that this thread is about that exact conversion. I'm working on it...lol
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    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?
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    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:
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    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
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    I admire your knowledge and determination. A great thread to read, best of luck with it
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    Quote Originally Posted by 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
    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
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    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
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    i dont think condensation is an important step here. it dosent matter if its saturated or not, i used 1g/1000ml concentration in my oraganic chemistry lab and it worked, but the trick is in choosing the solvent. the solvent should dissolve the solid in temperature higher than room temp (thus you boil it), in order to be able to recrystallize it again in regular room temp 30 c. I dont know if water is a good solvent (most androgens dont dissolve in water), alcohol maybe a better option, im not sure though because we used water to dissolve Benzoic Acid in my lab. i think the error comes from the choice of solvent, im not sure though maybe a more knowledgeable bro can comment on that.
    if you need help with the exact recrystallization procedure i have an experimental organic chemistry lab book with steps of recrystallizing many organic compound. i can copy the exact steps from the book if you wish.
    Last edited by x_muscle; 01-17-2004 at 09:25 PM.
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    Thanks for the offer but I know how to re-crystallize. I used the method that is on the first post of this thread. MeOH is the solvent, but many organic synthisis reactions are carried out at lower temps. The MeOH dissolves the Andro and the NaBH4 in an ice bath. Then the acetic is added to catylize the reaction. I have the mechanism posted a few posts up. You might have synthisized Nerolin, which is simmilar in technique to what I'm trying here. I don't think this reaction is an Sn2 reaction though. Any ideas you have are appreciated though, as you can see that my first attempt was a failure.
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    i synthesized naphthalene and Benzoic Acid, which is very similar to what you doing.....keep the good work bro, you are actually encouraging me study my chemistry. if i managed to get the materials maybe i will try it on my own
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    I did some more research today and found that NaBH4 degrades quickly in MeOH. It is rather stable in EtOH though. Would it be a good idea to attempt this reaction in EtOH? I also ordered 15g Mn (IV) oxide in case I need to redissolve my crude product in dichloromethane and treat it with Mn. That should oxidize the over reduced portion back to TNE. Does anyone have any suggestions or ideas about this?
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    More usefull info:

    "Chemoselective Reductions with Sodium Borohydride. Aldehydes vs. Ketones." D. E. Ward and C. K. Rhee, Synthetic Communications, 1988, 18, 1927-1933.

    Abstract: Aldehydes can be reduced in the presence of ketones by sodium borohydride in 30% ethanol in dichloromethane at -78 C. The selectivity is generally greater than 95%.

    "A General Method for the Selective Reduction of Ketones in the Presence of Enones." D. E. Ward, C. K. Rhee, and W. M. Zoghaib, Tetrahedron Letters, 1988, 29, 517-520.

    Abstract: Ketones can be reduced in the presence of conjugated enones by sodium borohydride in 50% methanol in dichloromethane at -78 C. The selectivity is generally excellent. In favorable cases the reaction can be carried out at room temperature in dichloromethane with acetic acid as catalyst.
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    stanozolol?


    HI...
    does anyone know the reaction to make stanozolol?
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    Quote Originally Posted by sicosico View Post
    or try doing this : from superior muscle:


    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.
    ok im interested in these two.
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