How many AS can one make from 1-test.......

[candle25]

Re: How many AS can one make from 1-test.......

Originally posted by spidey
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%

I was refered here by a member at another board. I have a thread posted about hombrewing and have been looking for a method to yeild EQ. Your method sound reasonable, however I have a few questions:
1) You list 2,4,4,6-tetrabromocyclohexa-2,5-dione as the reducing agent. Do you mean 2,4,4,6-tetrabromocyclohexa-2,5-dinone RN#: 20244-61-5?
2) Won't any brominated cyclohexane work regardless of Br positioning?
3) Myself and many others have been researching 1T for quite a while and not been able to locate a molecular formula or structural makeup. Where did you get your info on 1T?
4) Could you recomend any research sites other than ChemID, Chemfinder, or Steraloids.com?

Nice looking board BTW. I'll be sure to check out the chemistry section before I leave.

[spidey]

Re: Re: How many AS can one make from 1-test.......

Originally posted by candle25
I was refered here by a member at another board. I have a thread posted about hombrewing and have been looking for a method to yeild EQ. Your method sound reasonable, however I have a few questions:
1) You list 2,4,4,6-tetrabromocyclohexa-2,5-dione as the reducing agent. Do you mean 2,4,4,6-tetrabromocyclohexa-2,5-dinone RN#: 20244-61-5?
2) Won't any brominated cyclohexane work regardless of Br positioning?
3) Myself and many others have been researching 1T for quite a while and not been able to locate a molecular formula or structural makeup. Where did you get your info on 1T?
4) Could you recomend any research sites other than ChemID, Chemfinder, or Steraloids.com?

Nice looking board BTW. I'll be sure to check out the chemistry section before I leave.

1) Sorry, a little typo there but I can't go in and edit my post now. The compound is 2,4,4,6-tetrabromo-2,5-cyclohexadienone CAS# [20244-61-5]. Aldrich sells it for 5g/$34.40, catalog no. 30,238-4.

2) No, just any brominated cyclohexane will not work. The driving force for this reaction is the aromatization of the above reagent to 1,3,5-tribromobenzene by loss of a bromine.

3) The structural formula for 1-T is all over the place. I can't remember where I first saw it. You can buy the powder for pretty cheap from 1fast400.com. The structure might be there.....

4) I didn't use any of those research sites. All these syntheses are just out of my head; I am a Ph.D. synthetic chemist.

If you want to make boldenone, there is an easier way. I was trying to make everything starting from 1-test so the routes I gave may not be the easiest or most efficient as some things are more easily made from some other starting material.

Boldenone can be had in approximately 90% yield from 1,4-androstadiene-3,17-diol by just stirring the prohormone in dichloromethane with 5x weight equivalents of activated MnO2 for 24 hours at room temperature. Just filtering away the MnO2 after the reaction and evaporating the solvent gives pure boldenone.

[candle25]

Thanks Spidey! I'm glad to see that you're not bashful with your knowledge. The newer conversion you posted looks much better considering the theoretical yield. I have 30g of 1T from 1F400. No MSDS or such was provided. Here are the conversions I currently have:
Clenabutrin from powder
How to convert Androstendione to TNE
Orals from Powders
Oral D-Bol
Winstrol from Powder
Fina
4AD to Test Base
Boldenone Undeclynate to Equipoise
Testosterone Enanthate
Test Cyp + Enan to Testosterone
Tren Enanthate
Tren Acetate
Synovex to Test Prop

Do you have any others you would like to share? I've already searched this whole board.

[spidey]

Well, the only ones I can think of that do not take a lot of synthetic training are the MnO2 oxidations. They are easy and generally free of side reactions so pure product is obtained without the need to further purify it.

Any of the prohormones with either a 1,2 or 4,5 double bond (or both as in boldenone) can be oxidized in this manner to the corresponding steroid:

4-androstenediol --> testosterone
19-nor-4-androstendiol --> nandrolone
1,4-androstadiene-3,17-diol --> boldenone

You can buy prohormone esters like 4-androstenediol-cypionate and get test cyp in one step.

You can also get there from the dione prohormones like 4-androstenedione, 19-nor-4-androstenedione, and 1,4-androstadienedione by carefully reducing with NaBH4. The conjugated 3-one is harder to reduce so the 17-one can be reduced in its presence.

[bigkid]

one simple step?

I'm lost!

[bigkid]

Is this the place?

http://www.kilosports.com/productsall.cfm

[Core]

Re: Re: Re: How many AS can one make from 1-test.......

Originally posted by spidey
1)

Boldenone can be had in approximately 90% yield from 1,4-androstadiene-3,17-diol by just stirring the prohormone in dichloromethane with 5x weight equivalents of activated MnO2 for 24 hours at room temperature. Just filtering away the MnO2 after the reaction and evaporating the solvent gives pure boldenone.

Way to go spidey! This is excelent information! I've been trying to figure out a method of doing this for about a year now.

I do have a question though. I don't have your extensive chemistry background. I took a year of organic, analytical, and a quarter of bio back in college, but failed to get a minor because of an injury that made me drop one of my organic lab credits. I fealt that my additional chemistry credits had earned me that minor, but the University fealt otherwise. So bear with me if I say something stupid.

I'm curious as to what prevents a diol from becoming a dione in the above reaction. We are replacing the 17 carbon's ketone group with a hydroxyl group to change 1,4ADiol to boldeneone, I just don't see the mechanism that is protecting the 3 carbon's ketone from doing the same. I'd expect the resulting product to be 1,4ADione.

Does it have something to do with the proximity to the 13 carbon which has the 4 carbon bonds or 18 carbon crouding the 17 carbon's ketone?

I would just love to hear the explaination as to how this reaction is limited to only the 17 carbon.

Thanks spidey.

[candle25]

Bro, I'm glad to see someone with an intrest in the chemistry, but I'd advise against waisting your time on these type conversions. I tried many times without sucess. Just search untill you find a powder source and work with that. I never tried the boldenone conversion, but I'll look it over and see if I can help. BTW, Spidey hasn't been around for a while so I doubt that you'll hear from him.

[candle25]

OK. I think Spidey made a mistake. I couldn't find where you quoted him from, but in the quote he said to use 1,4-androstadiene-3,17-diol. I think he must have meant 1,4-androstadiene-3,17-dione. Here is the info on that compound:

Names and Synonyms

Name of Substance: Boldione
1,4-Androstadiene-3,17-dione

Synonyms
1,4-Androstadiene-3,17-dione
1-Dehydroandrostenedione
Androstadienedione
EINECS 212-977-2
NSC 49080

Systematic Name
Androsta-1,4-diene-3,17-dione

Classification Codes
Hormone

Formulas Molecular Formula
C19-H24-O2

Registry Numbers CAS

897-06-3

It looks like the 3 C Ketone is being protected by the double bonds on the 1,2 & 4,5 C.

Also as Spidey said, this makes the 3-OH an allylic alcohol. MnO2 selectively oxidizes allylic alcohols. I can't see where a 3-OH would ever be formed. The other double bonded O is where the chemistry takes place.

Some more info:

Boldenone
CAS# 897-06-3
MF C19H24O2

[Core]

Originally posted by candle25
OK. I think Spidey made a mistake. I couldn't find where you quoted him from, but in the quote he said to use 1,4-androstadiene-3,17-diol. I think he must have meant 1,4-androstadiene-3,17-dione. Here is the info on that compound:

<snip, snip>

It looks like the 3 C Ketone is being protected by the double bonds on the 1,2 & 4,5 C.

Also as Spidey said, this makes the 3-OH an allylic alcohol. MnO2 selectively oxidizes allylic alcohols. I can't see where a 3-OH would ever be formed. The other double bonded O is where the chemistry takes place.

Alright. It makes more since that we're dealing with the dione so the double bounds often help stabelize functional groups.

So you think it isn't worth trying, eh?

Hmm. I was thinking about trying this and then add an acetate ester to the resulting product.

I figure I could disolve the resulting powder in acetic anhydride with a light acid catalyst to generate boldenone acetate. Once the resulting substance is washed and dried I should see a measureable mass increase which would indicate the first chemical process worked. After all I wouldn't be able to generate the ester w/o succeeding in converting the 1,4dione into boldeone.

Any mass shortfall could be used to calculate rough yield.

What do you think? Am I insane?

[alcast082]

This is some funny shit, i feel like i am in my organic chemestry class, we actually covered alot of these synthesis in class but used common organic products instead of test and things like that.

[candle25]

Core, you are very bold to want to attempt a synthisis followed by an esterification. I don't think you will have any luck, but I will be glad to support you however I can if you want to attempt it. I am only a BS in Chem Engineering so I won't be as much help as Spidey would have been. Sigmund Roid was also very good at home chemistry but I haven't seen him in a while either. I wish we could post word documents here because I have the mechanism for many of these reactions drawn out using ISIS. I think you'd find them helpful. I tried the synthisis of Androstendione to TNE. There is a thread on it here somewhere. I got a crappy yield and the MP was terribly off for the desired product. Idealy one would need to do a synthisis of the crude product, then a purification, then an esterification. That is a lot of serious chemistry. Here is a method for esterification that Spidey and I came up with for TNE: (It should work for Boldenone as well)

Dissolve testosterone (10g, 34.7mmol) in 130mL dry dichloromethane. Add pyridine (8.4mL, 104mmol) and DMAP (424mg, 3.47mmol) and cool the solution to 0 deg C. While stirring at 0 deg C, add acetyl chloride (3.7mL, 52.1mmol) dropwise. Stirr at 0 deg C for 5 minutes and then allow the reaction to warm to room temp. The reaction is monitered by TLC to ascertain when it is complete (an hour or two maybe). The yellow solution is transfered to a separatory funnell with dichloromethane and is washed with 3 x 50mL saturated CuSO4 solution (to remove pyridine and DMAP).

1M HCl solution may be substituted for the CuSO4 solution but if it is, you must wash the organic layer with sat. NaHCO3 solution to remove acid.

The dichloromethane layer is dried over MgSO4 and the solvent evaporated to give testosterone acetate. It may be a little yellow but it is still good. If you want nice white stuff, a simple column (chromatography) can be used to purify your crude product.

I also have alot of Allumina TLC plates and MnO2 left from my experiments. I'd be glad to send them to you if you'd pay shipping. MnO2 is very expensive, so that would help you alot. Just let me know.

[Core]

Originally posted by candle25
Core, you are very bold to want to attempt a synthisis followed by an esterification. I don't think you will have any luck, but I will be glad to support you however I can if you want to attempt it. I am only a BS in Chem Engineering so I won't be as much help as Spidey would have been.

Hmm. If you couldn't pull it off with a BS in Chem Engineering, a hobbiest chemist like myself 10 years out of Univ isn't likely to get it right.

Sigh. :(

The esterfication after the synthesis would have been an attempt to verify the success of the synthesis. 1,4Adione -> Boldenone only increases the molecular mass from 284.3973 to 286.4132. Hardly a measurable change w/o an anylitical scale. The scale I use is only acurate to +/-0.05g optimistically speaking. Alternatively I do have a junky melting point aparatus but it is in pieces and is missing a thermometer and is probably unsalvageable.

I think more than one of us would be interested in seeing the reactions you've diagrammed.

If you can't export them to PNG format dirrectly, you could screen shot them and then crop the images with a a graphics editor. GIMP comes to mind if you lack Photo Shop. If it is not too much trouble, why not post them to this forum?

[candle25]

I would be glad to. How do you do a "screen shot"? I have great graphic editing software. Also, I've never heard of a PNG format.

[Core]

Originally posted by candle25
I would be glad to. How do you do a "screen shot"? I have great graphic editing software. Also, I've never heard of a PNG format.

PNG just stands for Portable Network Graphic. It is a common graphic format used on web pages. You could just as easily use GIF if you have software that can export that format as well.

A screen shot depends on the OS.

If you are on MS Windows you can create a screen shot by selecting the window you want to capture and then hit <ALT> <PRINT SCREEN>. This copies the window to your clip board. From there you can paist it into Word which I believe makes it a huge BMP file.

Normally I do this sort of thing from Unix and use "import" to capture a window to a graphics file. It has been a few years since I've done a screen shot from Windows, but people do it all the time so I know it still works.

If you are on a Mac, I don't know what you do. There has to be a way I'd think.