4AD to test base

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  1. DDD
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    Originally posted by rotarnomore
    Wanted to post a correction from my last post. The report is extremely confusing and I reread it again. Apperently the 4-AD and MnO2 are suspended in the chloroform and mixed for 10 hours. The report then states that the MnO2 is filtered and washed with chloroform and the chloroform is evaporated away. I'm not sure if the test remains in the MnO2 crystals or the chloroform. I would assume the filtered crystals contain both the Test and the MnO2 since neither should dissolve in chloroform. What doesn't make sense is the report then goes on to state that the test was crystallized by using the acetone-hexane mixture. This doesn't make sense because I would think the test WOULD dissolve in an acetone/hexane mixture but the MnO2 would not. I'm also assuming the chloroform was evaporated away to make sure that no test remained in solution so a final amount of total conversion could be calculated.
    I also wanted to add a word of extreme caution. Chloroform is a known carcinogen (cancer causing). It is also heavier than air and the vapors will concentrate near the floor. It can also make you pass out.
    Nice attempt but still wrong. I haven't even read the procedure and I've already figured this one out. I'll post the correct way to convert 4AD to Test via this technique, as well as how to reconstitute the Test, once my Karma have increased to a point where I feel it's time to post. So get adding them Karma. Yes, I know this sounds infantile. Oh well.

  2. DDD
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    Originally posted by maggmaster
    Wow triple d rather cutting without an interpretation, Im assuming you are a chemist and i will discuss with you on those terms. I am not a chemist but I do have some interest in the subject and have done some self study. Just dont shoot down people who are trying to do something cool for everyone.
    Big props for crazypete. If it weren't for his totally bastardized interpretation of a procedure, I wouldn't have been able to figure this all out. He gave me just enough info to break the puzzle apart and put it back together properly. Thanks crazypete!!!
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    Actually, I finally figured it out. Here is what happens:
    1. the reactants (4-AD and MnO2) are allowed to mix for 10 hours. The MnO2 crystals are then extracted with filter paper and they are washed with hot chloroform to remove any remaining test.
    2. The report then states that the chloroform is then evaporated to dryness. This was the part I was confused on. I believe water is formed in the reaction so the experimentors (is that a word?) evaporated the water out of the solution.
    3. The test was then crystallized using the acetone/hexane mixture.
    4. The report also states that a 2nd and third crop were extracted from the same solution giving a total of 90% conversion.
    Viola. All that and no karma
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  4. DDD
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    Originally posted by rotarnomore
    Actually, I finally figured it out. Here is what happens:
    1. the reactants (4-AD and MnO2) are allowed to mix for 10 hours. The MnO2 crystals are then extracted with filter paper and they are washed with hot chloroform to remove any remaining test.
    2. The report then states that the chloroform is then evaporated to dryness. This was the part I was confused on. I believe water is formed in the reaction so the experimentors (is that a word?) evaporated the water out of the solution.
    3. The test was then crystallized using the acetone/hexane mixture.
    4. The report also states that a 2nd and third crop were extracted from the same solution giving a total of 90% conversion.
    Viola. All that and no karma
    You're getting closer but not quite. By the way Manganese Oxide is Mn3O4.
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    a couple of things:

    1. pete is an idiot. his procedure was not bastardized, he copied the wrong one (see the first one in the paper). i could come up with many excuses (exams, etc.), but i ****ed up and should have paid more attention. that and i should have noticed that methanol would not work well to recrystalize as i have a background in the field. i guess that my ego got in the way and blinded me to the fact that it was wrong.

    2. manganese dioxide is used, says so in the paper, it is the first thing under the experimental section. also the reactions text i found the reference in had manganese dioxide listed.

    3. the ratios are 25 parts chloroform, 5 parts MnO2, and one part 4AD

    4. mixing is at room temp for 10 hours, one could extend to 2 days, but results would be similar.

    5. filter product and wash with hot chloroform.

    6. evaporate chloroform

    7. crystallize with acetone-hexane and filter and dry.

    this is what the correct part of the study says (no i didn't read the section pertaining to 4-cholestenone this time)

    the yeild is ~75% originally if your neat and ~90% after the third crop.

    other than the fact that i copied the wrong part of the paper (which was spot on), i made no mistakes. rotarnomore's synopsis is right and this is the correct procedure as outlined in the paper.

    in the intro to the paper it mentions using benzene, ethylene chloride or acetone as the solvent. does anyone have any comments about this.

    cheers, pete
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    First off crazypete is right with the details listed. Secondly, Manganese oxide is not Mn3O4. Technically, Manganese Oxide is MnO. The experiment calls for managanese DIoxide which is MnO2. manganese has several oxidation states including 2,3, and 4. MnO2 leaves managese in the +4 oxidation state and it will decompose over time. This why I guess the people doing the experiment decided to make their own. They even state that they could not find a reliable commercial source so they freshly prepared their own and left it in a flask with a stopper on it.
    In regards to the solvent question. The paper says that the 4-AD is suspended, not dissolved in the chloroform. The Manganese dioxide was then removed by filtration and washed with hot chloroform. " The article states "The combined chloroform [the washings of the MnO2] is then evaporated for dryness." It then says that "Crystallization from acetone-hexane yielded [testosterone]....". Why would you need to crystallize an already crystallized (since the chloroform was evaporated) product? One thing I don't understand from the report is why the chloroform is evaporated and then crystalized from an acetone/hexane solution. Why would you go through 2 crystalization processes? Anyone know? One more note on the carrier solution. I personally would rather use acetone. It is much less toxic and you can pick a gallon of it up from Lowes for about $10.
  7. DDD
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    Originally posted by rotarnomore
    First off crazypete is right with the details listed. Secondly, Manganese oxide is not Mn3O4. Technically, Manganese Oxide is MnO. The experiment calls for managanese DIoxide which is MnO2. manganese has several oxidation states including 2,3, and 4. MnO2 leaves managese in the +4 oxidation state and it will decompose over time. This why I guess the people doing the experiment decided to make their own. They even state that they could not find a reliable commercial source so they freshly prepared their own and left it in a flask with a stopper on it.
    In regards to the solvent question. The paper says that the 4-AD is suspended, not dissolved in the chloroform. The Manganese dioxide was then removed by filtration and washed with hot chloroform. " The article states "The combined chloroform [the washings of the MnO2] is then evaporated for dryness." It then says that "Crystallization from acetone-hexane yielded [testosterone]....". Why would you need to crystallize an already crystallized (since the chloroform was evaporated) product? One thing I don't understand from the report is why the chloroform is evaporated and then crystalized from an acetone/hexane solution. Why would you go through 2 crystalization processes? Anyone know? One more note on the carrier solution. I personally would rather use acetone. It is much less toxic and you can pick a gallon of it up from Lowes for about $10.
    Sorry your right, Manganese Oxide is MnO, I was looking at Manganese Manganic Oxide Mn3O4. Either way, neither is soluble in chloroform but 4-AD and Test are soluble in chloroform. Technically, you could just evaporate the chloroform after filtering and you would be left with Test. If you were in a hurry you could mix an equal amount of methanol or methanol/acetone with the chloroform/Test solution. You could then recrystalize by adding/mixing your chloroform/alcohol/Test solution with an equivalent amount of distilled water (while mixing on a magnetic stirrer or getting real aggressive with a glass stirring rod) and the Test will then precipitate out and can be filtered off. The amount of chloroform used could be reduced or certainly much more 4-AD used in the same volume of chloroform. The manganese dioxide could be reduced as well but the reaction time would be slower then. MnO2 should be added in excess though.
    Last edited by DDD; 06-17-2003 at 12:25 AM.
  8. DDD
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    Originally posted by crazypete
    a couple of things:

    1. pete is an idiot. his procedure was not bastardized, he copied the wrong one (see the first one in the paper). i could come up with many excuses (exams, etc.), but i ****ed up and should have paid more attention. that and i should have noticed that methanol would not work well to recrystalize as i have a background in the field. i guess that my ego got in the way and blinded me to the fact that it was wrong.
    Hey, that's alright. I'm sure everyone would have gotten great results from the Manganese Oxide transdermal they could have made from your original posting. We all make mistakes.
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    i think the second crystallization is done to make sure all the chloroform is removed from the solid, then you can filter, wash and dry. just my thoughts. i like the idea of using acetone to run the reaction.

    cheers, pete
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    Originally posted by crazypete
    i think the second crystallization is done to make sure all the chloroform is removed from the solid, then you can filter, wash and dry. just my thoughts. i like the idea of using acetone to run the reaction.

    cheers, pete

    I thought of this myself because I have seen it done in other experiments as well. It sure did make the report confusing. One question for ya. How in the heck did you come across this article? Like I said in my original post I don't use steroids myself but after looking at all the views this post got, I'm thinking of investing some money in MnO2 production
  11. DDD
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    Originally posted by crazypete
    i think the second crystallization is done to make sure all the chloroform is removed from the solid, then you can filter, wash and dry. just my thoughts. i like the idea of using acetone to run the reaction.

    cheers, pete
    Evaporation is how the chloroform is removed. It evaporates with no residue left behind. I think the reason the Test is recrystallized is because it's welded to the bottom of a petri dish after evaporating the chloroform with heat. The Test is redissolved in the acetone/alcohol. The most common technique of crystallizing any roid from alcohol and/or acetone is the addition of distilled water followed by filtration of the product which precipitates out. Air dry on the filter.
  12. DDD
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    The reaction is run in chloroform because it doesn't react with the MnO2. The methanol does react with MnO2 and would use it all up, leaving none left to react with the 4-AD.
  13. DDD
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    Acetone and Alcohol are used for the recrystallization since they
    1. Both dissolve Test
    2. Both dissolve water
    3. Test doesn't dissolve in water

    The Test is dissolved in Acetone/Alcohol. Water is added with stirring. The Test crystallizes out of solution. Filter and air dry. Pretty simple.
  14. DDD
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    Originally posted by DDD


    If you were in a hurry you could mix an equal amount of methanol or methanol/acetone with the chloroform/Test solution. You could then recrystalize by adding/mixing your chloroform/alcohol/Test solution with an equivalent amount of distilled water (while mixing on a magnetic stirrer or getting real aggressive with a glass stirring rod) and the Test will then precipitate out and can be filtered off.
    By the way, this is a pretty half-ass short cut. I wouldn't do it this way because your Test recovery % would probably be lower. The chloroform is a very heavy solvent and would begin to phase separate once the water was added and the chloroform would redissolve some of the Test once this phase separation happened. You could recover it though by evaporating the chloroform once you were done filtering your Test that did settle out. Doing it this way would be more work in the long run, but a quicker way of recovering some of your Test.
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    rotarnomore: i got the reaction from a book full of steroid reactions from thode library at mcmaster university. many such texts exist and have references to the original paper which one can go look up in the journal stacks. you have to go to a university with a good science program, they will have the good stuff in the library. it is probably not commercially feasible to produce MnO2, only worthwhile for personal use if you have the time and knowledge otherwise just buy it or buy the raw material you want. someone will make it for cheap, probably in china. but hey that's the chemical industry the only way is to do it big.

    DDD: you game for working out more advanced procedures?

    cheers, pete
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    Is this economical ???


    Just a simple question for our chemistry experts regarding the economics of this process:

    test base (98%) can be purchased from china from anywhere from $.60 to $2.50 per gram. Test prop can be made from synovex from around $7.00 per gram. With those numbers in mind, is it economical (ignoring the question of whether these products are accessible to the masses) to be able to produce test from 4-ad given the cost of the chemicals and the lab equipment required to produce it?

    Thanks
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    100g 4AD $90
    500g MnO2 $40
    2500ml or 2.5L chloroform $164 (can be had cheaper)
    4L acetone $42
    distilled water cheap as hell
    isopropyl alcohol 99% $6/L
    stirrer/heater $100
    glassware $50

    using you're own homebrew: priceless

    total ~$400/75g test base

    so $5.33/g and you know its the stuff and subsequent batches are even cheaper

    cheers, pete
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    i don't care much to deal with the heat that comes with illegal test base from china, if i wanted to, there are plently of companies that will sell a kilo for less than $500 US, also you could get boldenone, nandrolone, tren bases or any ester etc...

    i'm sure i would have no problem getting it. just go through eastern europe and then to europe and on to canada. risk is minimal if you're not an idiot and you can make a killing. would i risk my future just to get cheap ****, hell no. wait a minute i've never even used any. the point is you're not going to get it much cheaper than $5/g unless you know someone. so now we have a low risk way to do it. 3 ten week cycles with 1g per week absorbed for $500 if you use transdermal, add in 1-T and you're laughing.

    next week, how to make boldenone base from 1,4ADD, unless it can be had for cheap, in which case i won't bother.

    cheer, pete
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    Has anyone done the conversion yet?


    Has anybody done the conversion yet? If so, what were the results?
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    yeah, back in '53. 90%. sorry, couldn't resist. i don't know if anyone has tried this recently.
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    Does anyone wanna summarize the method..
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    Originally posted by crazypete
    yeah, back in '53. 90%. sorry, couldn't resist. i don't know if anyone has tried this recently.
    The reason that I asked whether anyone has done this procedure and what were the results is that there has been a tremendous amount of discussion on this thread as to how it should be done, what chemicals required, etc., etc. but so far no one here has done it.

    I'm not disputing the fact that it was done in 53 when the procedure was published. I just want to know if anybody with the knowledge and materials to do it are going to step up to the plate and then do it. Otherwise, this discussion will continue to remain just that - a lively debate on how to make test from 4-AD. I mean this thread is several months old!!!

    Personally, I do not have the skills nor the chemicals to try this. And, having read some of the statements here regarding the toxicity and flammability of some of the materials, I don't think I would consider it until one of our "experts" has tried it (and that would include testing the product for purity and possibly even administering it to themselves).

    So, all I am saying is that if you believe that it can be done safely and economically, then do it and let us all know how it worked out, and more importantly what you learned from the process.
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    well said. i'd like to give it a go, i think that i'd be able to test the material produced at school, they have the right equipment in the lab. i doubt i'd be able to do it before the end of the summer though.

    cheers, pete
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    Just posting so I can subscribe to this thread. I work in a lab so getting these chems will be no problem. I love this place....lol
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    OK bro's, I have a few questions about this process.
    1) What is the ratio of acetone/hexane used to re-crystallize the test?

    2)During re-crystallization are the only things used acetone/hexane? I can't find much on the solubility of Test, but one source said it was around 26g/L. If so you wouldn't be able to wash the final product with water.
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    sars was blown up by the media man, I know somebody who had it before it was all over the news, he was in my english class, he recovered from it no problem.
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    This is my understanding of the process. I've just organized the entire thread to an easy to follow article. I'm still not exactly sure about what ratio of acetone/hexane to use. If anyone knows, please post it up. Also keep in mind that no one has done this and posted results.Here's the article:

    Abstract:

    4-androstene-3,17-diol (4AD) undergoes an oxidation/reduction to form 4-Androsten-17-ol-3-one (Testosterone).

    Introduction:

    This is just a summary of a conversion found at AM. The original idea was published in the Journal of the American Chemical Society, 75th Ed. , Sondheimer et al. 1953. Also thanks to Crazypete for digging it up and rotarnomore for contributing. I have simply organized the process and added some useful information.

    Most of this process is conducted at room temperature. However, during the evaporation process be aware that Hexane is highly flammable. Also note that Chloroform is somewhat poisonous and its vapor is heavier than air. If inhaled for a long period it can cause you to pass out. It is advised to conduct this process in a well ventilated area.

    Reagents...................... ..MF................MW........ ..MPC.........BPC
    Chloroform.................... ...CHCl3...........119.3779... ..N/A......61.7
    Acetone....................... ....C3H6O..........58.0798.... .-94.3.....56
    Hexane........................ ....C6H14........86.1766....N/A.............
    Manganese Dioxide.............MnO2...... ........86.9368.....535....... .N/A
    4-Androstene-13,17-diol....C19H30O2.....290.44... ......................
    4-Androsten-17-ol-3-one....C19H28O2....288.4...... ......154.........


    Discussion:

    C19H30O2 + MnO2 ---> C19H28O2 + MnO + H2O
    (Molecular Formula for Reaction)

    In this reaction MnO2 is used as an oxidizer to remove the two H from the single O at the end of the hexane ring. MnO2 is also the excess reagent in the reaction. Chloroform acts as the solvent for the 4AD & the Test because it will not dissolve the MnO2 or MnO.

    Experimental:

    Supply List:

    Couple of 500ml beakers
    Magnetic Stirring bars
    Stir/hot plate
    Thermometer
    Filter papers
    Filter funnel
    500ml Filter flask
    Thick walled hose
    Scales
    *Most of this can be replaced with a variety of things….be creative.

    Reagents:

    *To make 1g 4-Androsten-17-ol-3-one (Testosterone) you’ll need:
    25-100ml Chloroform
    5-10g Manganese Dioxide
    1g 4-Androstene-13,17-diol (4AD)

    Procedure:

    •Pour chloroform in a beaker equipped with magnetic stirring bar.

    •Begin stirring and add in 4AD & MnO2. Allow mixing to proceed for a minimum of 10hrs. at room temperature.

    •Filter the solution and wash the solid 3 times with warm chloroform. Save the washes and combine them with the filtered solution.

    •Evaporate the chloroform using the hot plate &/or a hair dryer until it is completely dry.

    •Allow the beaker to cool to prevent shattering it. Then add an acetone/hexane mix to re-crystallize the Test.

    •Filter solution and dry the crystallized Test. Save the acetone/hexane soln.

    •Let the Test air dry in a desicator jar or lightly covered with a paper towel.

    •Weigh the crystals. If you have around 90% yield then you’re done. If not, filter the acetone/hexane soln again and repeat drying/weighing process. Continue doing so until you have a 90% yield.
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    great post candle
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    Quote Originally Posted by Klaus
    It's not Manganese Dioxide; it's Manganese(IV) Oxide.
    What are you refering to bro? The reducing reagent is MnO2 with an oxidation charge of +4 (O has a charge of -2 x 2). MnO would put Mn in the +2 state.
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    from where you will get hexane?
    i belive its a aromatic or cyclo molcule.....most cyclo agents are toxic (not all). although im not sure hexane toxic or not. i dont want any left over from crystalization to enter my body. i will hesistate to put hexane in my body.
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    Quote Originally Posted by x_muscle
    from where you will get hexane?
    i belive its a aromatic or cyclo molcule.....most cyclo agents are toxic (not all). although im not sure hexane toxic or not. i dont want any left over from crystalization to enter my body. i will hesistate to put hexane in my body.
    I spoke to Chemo about this process & he said that Test isn't sol in water to any large degree. In light of that, it should be OK to wash the final product a few times with DI water. That should remove any residual compounds. A simple melting point test should is a rough way of determining purity (Unless you have access to an NMR or such).
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    Quote Originally Posted by Klaus
    MnO2 is an ionic compound, not a molecular compound. Calling it Manganese Dioxide is incorrect nomenclature. The Manganese atom must have a 4+ charge since it is bonded with two oxygen atoms. Since this is so, it is correctly called Manganese(IV) Oxide. The (IV) denotes its charge.
    Manganese dioxide [1313-13-9]
    Synonyms: Black Dioxide; Black manganese oxide; Cement black; Manganese dioxide; Manganese Black; Manganese (IV) dioxide; Manganese (IV) oxide; Manganese oxide; Manganese Peroxide;

    I'm not really following what you're saying. I recall back in inroductory chem when we learned nomenclature, MnO2 was called manganese dioxode. Unless someone changed chemistry without telling me, it's still the same. I happen to work at a facility where MnO2 is produced occasionaly as an impurity. The kenetics to form MnO2 are very good in a Mn solution at a pH of =<7. Now when I have to discuss this with our chem E's in Germany, we universaly recognize it as manganese dioxide. I see what you are saying, but in real life you'll never hear anyone refer to manganese (IV) oxide.
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    For what its worth, Manganese Dioxide is correct nomenclature. Hexane is neither cyclic nor aromatic but is aliphatic (straight chained). It is still toxic but to what level I'm not exactly sure. I wouldn't think a small absorbtion would be any worse than spilling gas on your hands. You can Material Safety Data Sheets (MSDS's) on the web if you do a search.
    Chris
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    update? anyone actually done this yet or is it still just discussion?
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    Quote Originally Posted by Crow Magnum
    update? anyone actually done this yet or is it still just discussion?
    Id like to know that as well, also is the MnO2 active did anyone find that out yet?
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    Quote Originally Posted by Mr.Striation
    Id like to know that as well, also is the MnO2 active did anyone find that out yet?
    I don't think there is such a thing as "inactive" MnO2 (or active for that matter). I read the experiment and my guess would be that the scientists that conducted the experiment had a batch of MnO2 go bad on them (probably oxidizes itself in air to MnO which is a more stable state for Manganese). they stated that a freshly prepared batch of MnO2 worked much better. the experiment only relies on the Mn in the +4 oxidation state.
    Chris
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    That is correct rotarnomore. I have personally given up on these type conversions. I have plenty of MnO2 if anyone wants to seriously try this. I also have Alumina TLC plates. Shoot me a PM if anyone is interested. All I'd ask is that you pay shipping and that you post your test procedures and results.
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    Quote Originally Posted by candle25
    That is correct rotarnomore. I have personally given up on these type conversions. I have plenty of MnO2 if anyone wants to seriously try this. I also have Alumina TLC plates. Shoot me a PM if anyone is interested. All I'd ask is that you pay shipping and that you post your test procedures and results.
    What kind of test results would you be looking for?
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    Mr S: I'd just like to see how things go with his experiment.

    ps2: You can't use NaOH because it is most likely to dissociate as Na+ OH-. In this reaction MnO2 is used as an oxidizer to remove the two H from the single O at the end of the hexane ring. MnO2 is also the excess reagent in the reaction. Chloroform acts as the solvent for the 4AD & the Test because it will not dissolve the MnO2 or MnO.
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    why couldn't some saturated NaOH in methanol (similar to jweave23's synovex procedure) do it?
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