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Andro to TNE...Spidey??

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  • Andro to TNE...Spidey??

    How to convert Androstendione to TNE

    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
    Androstenedione (powder)
    Methanol (wood alcohol)
    Sodium Borohydride (sodium tetrahydroborate)
    Acetic Acid (ethanoic acid)
    Distilled Water
    Litmus Paper
    Thermometer (Fahrenheit)
    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).


    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.
    The cloudy precipitate that forms is filtered off and the filter cake is washed extensively (several times) with water.

    9)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.

    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.


    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.

  • #2
    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.

    Comment


    • #3
      That's why I posted this. I knew you'd have some great idea! Do you know of a place online that I can read the Journal that you mentioned? I'd like to compair the process and see if there are any other differences. Also -78C (-108.4F) seems like it would be hard to maintain. Any ideas on that other than an ice/salt bath?

      Comment


      • #4
        Go to your local university chemistry library and look it up there. It's a very common journal and any such library would carry it. You could try searching PUBMED for it. The authors are Dale E. Ward and Chung K. Rhee. The title of the article is "Chemoselective reductions with Sodium Borohydride".

        -78 deg C is not hard to maintain. That is the temperature of a dry ice/acetone bath. You will find that is a fairly common constant temp bath used in synthetic chemistry. Ice/salt baths can only get down to about -20 deg C (and even then it is tricky).

        Comment


        • #5
          I'm a student at a great university with such a library. It's just such a long drive. As for the acetone/dry ice bath, I can get the acetone for free, but the dry ice is another story. I'll search the internet and see if I can find a supplier. I have an account with Fisher & Acros as well.

          Comment


          • #6
            you might try to look up gas suppliers in the yellow pages. We get ours from a company called Airgas dry-ice

            Comment


            • #7
              OK, I have all my supplies but dry ice. I called our gas supplier just now and BOC doesn't carry dry ice. However, they do carry liquid N. 180L for $40. My salesman said he'd loan me a 6' SS hose and diffuser to transfer it with. I have a 4L SS beaker I was thinking of doing the reaction in. I'm not really liking the idea of sinking another $40 in this project. What type of results do you think I'd have if I used a salt/ice bath? In all honesty, this conversion is highly impractical. I get all these chems free, but for soemone who doesn't it would cost out the a$$.

              Comment


              • #8
                Liquid N2 is way too cold. It will just freeze everything solid.

                Try http://www.dryicedirectory.com/ . Just type in your area-code at the top and it will tell you if there is anyone in that area-code who sells dry-ice.

                It shouldn't be that hard to find. It's used for many legitamit projects from making your own root-beer to making fog special effects in your jacuzzi.

                As for the chemistry costing a lot, not if you consider that for a hundred bucks or so you can buy enough reagents to make kilograms of material.

                Comment


                • #9
                  BTW, you could just do the reaction at warmer temperatures. You will get a larger amount of the over-reduced diol but you can take that crude product mixture and dissolve it in dichloromethane and add 5x by weight of MnO2. Stirr for 24 hours at room temp and then filter off the MnO2. That will oxidize any diol to the 3-keto-17-ol steroid.

                  Comment


                  • #10
                    Thanks for the link spidey. I found a supplier very close using it. It's dirt cheap too. $0.93/lb at a 6lb minimum. So I'm going to pick it up tommorrow and get this thing started. I'm only going to have to maintain the low temp for about 1hr so I don't think that will take much. I have 60g of andro so I'll prob do several batches just to get used to the process. One thing I'm concerned about is the glassware I'll be using. Do you think it will withstand the low temp? I use kimax and pyrex beakers from fisher. Also, I overlooked the fact that I need methylene chloride. I'm going to go by the hardware store and look at paint strippers. Would that be a bad idea?

                    Comment


                    • #11
                      Originally posted by candle25
                      Thanks for the link spidey. I found a supplier very close using it. It's dirt cheap too. $0.93/lb at a 6lb minimum. So I'm going to pick it up tommorrow and get this thing started. I'm only going to have to maintain the low temp for about 1hr so I don't think that will take much. I have 60g of andro so I'll prob do several batches just to get used to the process. One thing I'm concerned about is the glassware I'll be using. Do you think it will withstand the low temp? I use kimax and pyrex beakers from fisher. Also, I overlooked the fact that I need methylene chloride. I'm going to go by the hardware store and look at paint strippers. Would that be a bad idea?
                      I sort of doubt you will find paint stippers that are pure dichloromethane. Do you have access to chloroform? That will work as well but you must remove the ethanol which is used to stabilize it first. That is easily done by washing the chloroform with 3 portions of water in a separatory funnell and then drying the chloroform over MgSO4.

                      Comment


                      • #12
                        I happen to have chloroform but I have no MgSO4...lol. It looks like I'll have to wait untill I can get the methylene chloride. I could call my old Chem teacher and ask to buy what....half a L? I'd have to have a good reason for needing it and I really can't think of one.

                        Comment


                        • #13
                          Actually, I made a bit of an error here I think. I was thinking you needed the methylene chloride for the MnO2 oxidation but you are going to use it in the NaBH4 reduction, right?

                          Chloroform WILL NOT work in the NaBH4 reduction and may even be dangerous. Chloroform forms carbenes quite readily under basic conditions which are very reactive.

                          As for how much dichloromethane you need, read that paper and keep the ratio of dichloromethane to 4-AD the same in your reactions. Do the calculation on how much 4-AD you want to reduce and then you will know how much solvent is needed.

                          Oh yeah; the kimex and pyrex glassware you have will stand up fine to -78 deg C. Do you have a magnetic stirrer?

                          Comment


                          • #14
                            It may be easier and cheaper to do this at warmer temps the way you originally planned (but with excess NaBH4) to get your mixture of diol and test and then submit the whole lot to MnO2 oxidation overnight with 5x by weight MnO2. This will oxidize all the diol to test.

                            Comment


                            • #15
                              I'm not doing the 4AD conversion, we talked about that on a different thread. I'm doing andro to TNE. As far as I know MnO2 isn't needed. The very first post on this thread outlines what I'm attempting in detail. So are you saying I need MnO2? If so I have about 2g of Mn (IV) oxide. That's the same thing I think.

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