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Is there a method to convert 1,4 Andro to Boldenone base?

Hey again Growmore,

I like the idea of a filtration through MgSO4. Does filtration through magnesium sulfate or siliceous earth have intrinsic properties that pick up Mn or is it just good filter media? If it does pick up Mn would the rest of the MnO2 have to be reacted before hand? I assume there wouldn’t be any H2O present when skipping the acid extraction.
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I could be wrong, but I dont thing MgSO4 has any special affinity for Mn. The principle here is that its very hydroscopic, so after you do the acid wash and have Mn dissolved in your acid/water layer, you'll pull all of that out by filtering through MgSO4, because it will absorb all of the water left in the DCM.

Would it be possible to rinse solidified crystals with an HCL solution for a purification step?
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I don't think it would be necessary...after you've washed and filtered 3x times I think you're product would be as pure as its going to get, the only step left being proper evaporation/crystal formation.

I noticed Et2O mentioned as a solvent, it seams that this would be relatively difficult to come by; has anyone come across any other more viable options?
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Et2O isnt something you'd want to use in your kitchen. Fumes are heavier than air and extreemly flammable, so they could actually sink through the floor, flow into your basement and blow up your house afte they ignite of the pilot light on your furnace. You know those news stories that pop up from time to time where meth-labs out west just spontanously explode? Well, those guys are playing with Et2O in an unsafe environment!

DCM and Chlorform seem to be the best options here, and are relatively easy to obtain.

Hey Dr.D -

The inital result of this process would be the base form of our target hormone, right? (test base, boldenone base, etc) So would washing with dilute H2SO4 convert it to its sulfuric acid salt? I know this would be the case with base alkaloids. If so, would the salt-form have any effect on transdermal delivery? If the hormone does convert to an acid salt, does it become water soluble as well? Or, does the ease of converting alkaloids from acids to bases and vise versa not apply to hormones because they lack nitrogen?

Thanks Dr and BV for all of the great posts so far, I’ll be ½ to a degree after deciphering all this chem. talk
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:)Trying to wade though all all this info makes me wish I had majored in Chem.

BV
 
BigVrunga said:
I could be wrong, but I dont thing MgSO4 has any special affinity for Mn. The principle here is that its very hydroscopic, so after you do the acid wash and have Mn dissolved in your acid/water layer, you'll pull all of that out by filtering through MgSO4, because it will absorb all of the water left in the DCM.
BV
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This is what I had thought, just wondering how this would also possibly prove effective skipping the acid extract if your sample was pure enough (not cloudy) after paper filtration as Doc mentioned; I'de assume you'd still have to stir H2O2 into your solution with this type of purification (both to provide H2O as well as to reduce the residual MnO2)?

BigVrunga said:
I don't think it would be necessary...after you've washed and filtered 3x times I think you're product would be as pure as its going to get, the only step left being proper evaporation/crystal formation.
BV
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I was actually wondering if this might be a more simplistic alternative, although the full acid extract seams simple enough if you knew the proper ratios for the chem's used...

BigVrunga said:
Hey Dr.D -

The inital result of this process would be the base form of our target hormone, right? (test base, boldenone base, etc) So would washing with dilute H2SO4 convert it to its sulfuric acid salt? I know this would be the case with base alkaloids. If so, would the salt-form have any effect on transdermal delivery? If the hormone does convert to an acid salt, does it become water soluble as well? Or, does the ease of converting alkaloids from acids to bases and vise versa not apply to hormones because they lack nitrogen?
BV
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Definitely a good question?
 
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BigVrunga said:
Hey Dr.D -

The inital result of this process would be the base form of our target hormone, right? (test base, boldenone base, etc) So would washing with dilute H2SO4 convert it to its sulfuric acid salt? I know this would be the case with base alkaloids. If so, would the salt-form have any effect on transdermal delivery? If the hormone does convert to an acid salt, does it become water soluble as well? Or, does the ease of converting alkaloids from acids to bases and vise versa not apply to hormones because they lack nitrogen?

BV
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No, it wouldn't form the salt. You are right about nitrogen, this is an ionic bond w/ alkaloids and acids, just like a mineral salt such as Na+Cl-. There is no real bond, just an ionic attraction. The SO4 salt of a steroid could be made, and a lot of corticoids are made into PO4 or suc. or SO4 salts just for the water solubility advantage. A salt would not work in a trans, at least not a regular formula, but maybe w/ a DMSO/water mixtute. The most interesting thing about this would be it's potential w/ non-17-alkylated hormones to improve oral bioavailability. It's been done and patented w/ DHEA that I know of. It would actually be bonded though to the SO4 so the steroid would be a H or Na salt of the sulfated steroid. Anyway, the intermediate would still have the 17-methyl in place, so it would not be the base hormone, if I understand your question right. Only the 3 position would be affected. With an H2O2 reaction method, water and DBall would be the only reaction products.
 
No, it wouldn't form the salt. You are right about nitrogen, this is an ionic bond w/ alkaloids and acids, just like a mineral salt such as Na+Cl-. There is no real bond, just an ionic attraction. The SO4 salt of a steroid could be made, and a lot of corticoids are made into PO4 or suc. or SO4 salts just for the water solubility advantage. A salt would not work in a trans, at least not a regular formula, but maybe w/ a DMSO/water mixtute. The most interesting thing about this would be it's potential w/ non-17-alkylated hormones to improve oral bioavailability. It's been done and patented w/ DHEA that I know of. It would actually be bonded though to the SO4 so the steroid would be a H or Na salt of the sulfated steroid. Anyway, the intermediate would still have the 17-methyl in place, so it would not be the base hormone, if I understand your question right. Only the 3 position would be affected. With an H2O2 reaction method, water and DBall would be the only reaction products.
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Thanks for clearing that up, Dr.D. So, creating an acid salt out of a steroid molecule is a lot more involved than just mixing the freebase with an acid.

I think we've got pretty much everything covered for the MnO2 oxidation of diols to work - from the initial reaction through purification of the final product. Nice!

BV
 
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I go on vacation for a week (physical this time), and when I return, it looks like we have Wolfgang Puck and Julia Childs aboard.

If I may, re-enter this discussion post-hiatus.

Steroid molecules don't have free base forms in the way that cocaine or some other commonly encountered amine does. The term 'test base' is abused by BBers and is chemically incorrect. Now, I'm not with the chemical police and frankly don't care if "test no ester" is called test base, test acid, Silvia or Bob. It irritates me when guys talk about which test esther is best, but I let it go. Anyway, it would be incorrect to say that test and dbol are not 'acidic' or that they do not participate in acid/base reactions. However, with the exception of stanozolol and other steroids with nitrogen heteroatoms (such as pyrazoles, imidiazole, etc) steroids such as test, dbol, primo, DHEA, 4-AD,... are not significantly acidic, do not readily participate in acid/base reactions; in fact, they completely inert to even the "strong base," NaOH (in acid base reactions). This is in contrast to estradiol, where the aromatic A ring furnashes an alcohol (phenol) that is appreciably acidic. The less compromising alcohol group on androgens at C17 is unsaturated ("allicyclic") and (alone) is effectively never in such a form whereby the term 'test base' is accurate.

The discussion on sulfonated androgens is interesting.. The dogma here is that the improved bioavailability could(?) come at the cost of (much) higher elimination rate. On the other hand, the more soluble brand of the hormone could have some..interesting periferal effects. But hey fellas, don't you think we should first master the egg before we go for the filet?


Andy
 
DR.D said:
If a Whatman low ash filter would work, and I think it would, that would be fine.


Especially if you want to collect the Mn and use it again.
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For this reaction to work well, the oxidant needs to be gound (well) into a very fine powder which makes subsequent filtration steps at the end of the reaction problematic. I doubt that successive filtrations would be able to do the job...

Centrifugation really is the only way to go...

(why the long faces all the sudden? Who needs to buy a centrifuge when we've got Walmart appliance section, duct tape, and religeously recorded Mcguyver VHS library?)




I'm quite frugal in my chemical mindedness as well... But in this case, the oxidant is effectively spent :) You could re-charge the reduced product with permanganate.. if materials are scarce.. otherwise, it probably wouldn't be worth the effort to reserect your oxidant.
 
Andy13! Nice to have you back bro:) How was vacation?:)

The discussion on sulfonated androgens is interesting.. The dogma here is that the improved bioavailability could(?) come at the cost of (much) higher elimination rate. On the other hand, the more soluble brand of the hormone could have some..interesting periferal effects. But hey fellas, don't you think we should first master the egg before we go for the filet?
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Yeah, the egg first...

For the reaction to work well, the oxidant needs to be gound (well) into a very fine powder which makes subsequent filtration steps at the end of the reaction problematic. I doubt that successive filtrations would be able to do the job...
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Isnt MnO2 a very fine powder to start with? Or, are there varying grades of coarse/fineness?

Centrifugation really is the only way to go...
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What about the MnO2 extraction with H2O2 and dilute H2SO4? Your comments on that...?

(why the long faces all the sudden? Who needs to buy a centrifuge when we've got Walmart appliance section, duct tape, and religeously recorded Mcguyver VHS library?)
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Is it possible to build a centrifuge out of a VCR and old McGuyver tapes?:) Got any plans?

[/quote]
I'm quite frugal in my chemical mindedness as well... But in this case, the oxidant is effectively spent You could re-charge the reduced product with permanganate.. if materials are scarce.. otherwise, it probably wouldn't be worth the effort to reserect your oxidant.
[/quote]

Well, that is good to know. Reagent MnO2 seems to be relatively cheap, though.

Thanks for adding to the discussion, Andy13!

BV
 
BigVrunga said:
Is it possible to build a centrifuge out of a VCR and old McGuyver tapes?:) Got any plans?
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That'd be an interesting DIY project;) I havn't run into those plans unfortunately, but I did come across a little blurb about using an old tape player and a bar magnet to build a cheap magnetic stir; might as well go McGyver while playing chemist:D
 
Of course, all of this discussion is purely theoretical! Its purely an exchange of knowledge between responsible adults.

Dr.D or A13 - so do you think physical separation of the MnO2 from the DCM/steroid solution is necessary, or will the H2O2/H2SO4 extraction do the trick?

BV
 
BigVrunga said:
Of course, all of this discussion is purely theoretical! Its purely an exchange of knowledge between responsible adults.

Dr.D or A13 - so do you think physical separation of the MnO2 from the DCM/steroid solution is necessary, or will the H2O2/H2SO4 extraction do the trick?

BV
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Filtration through regular lab paper (IMO) probably won't cut it.. Repeated filtration sessions will cost you some product..

I think centrifugation would be ideal, but it certainly isn't the ONLY practical separation method.

For myself, chemical separation is a last resort. Actually, if I absolutely could not separate the mixture by physical means, I would probably look for different reaction scheme that has a more friendly workup.

If it were my project, I would probably attempt to separate the mixture with the following procedures:

1) Centrifugation!

2- Whatman filtration paper-- if this fails, and I think it will, the next thing to try would be a fritted funnel.

3)- filtration through celite

4) " " silica
5) " " alumina
6) " " maybe molecular sieves


I'm sure the submicron filters would work.. On the other hand, it would be such an inefficient process because of clogging.. If you thought fina clogged those filters.. just see what this stuff will do.

I'm pretty confident that the celite will take care of the Mn species.. If not, silica certainly would..

$20 for a sustanon amp is looking better and better :)
 
Just solubilize it, as I suggested, and extract. Then the filtration method is just secondary and not even really needed. Run the DCM through a drying column of MgSO4, anhydrous or a fluted whatman filter paper loaded w/ siliceous earth, and be done with it. You can use oven dried epsom salt if that's all you have. 20 bucks an amp isn't bad unless you know better. If you can master these do-it-yourself tricks, 20 bucks seems ridiculously expensive compared to home brew reagent costs!
 
Even though 'real' gear is readily available - Its way more appealing to me to gain some knowledge out of researching and performing an experiment like the one were discussing. After all:

Magnetic Stirrer $50
MnO2: $20
DCM: $10
Diol of choice $30

Being able to synthesize boldenone base in the comfort of your own home:
Priceless :drunk:


BV
 
So did anyone end up doing this?
 
I once had an imaginary friend that thought about doing it in a dream once if you know what I might be saying and the MnO2 granular using M14 worked great when spun for a week using the method I recommended. Of course, I scolded them and told them to never speak of it again or I would have to put the spank down on it big time. Does that make any sense?
 
No
 
DR.D said:
OK, fair enough. PM me for the whole story :cool:
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Thank you sir :wave:
 
DR. D can you use the same process with a 4-AD cypionate and use the cypionate for protection on the 17 OH group or will the oxidation screw the ester up.
 
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almcdon said:
DR. D can you use the same process with a 4-AD cypionate and use the cypionate for protection on the 17 OH group or will the oxidation screw the ester up.
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Yes, you can use it juuuuust fiiiiiiine! The ester remains in tact. :thumbsup: (that's in my best Mr. Hankey voice)
 
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