Extracting estradiol from pellets-- my method.

[Andy13]

Crush pellets, stir in toluene, filter. Remove powder from filter, stir in toluene some more, filter. To the combined toluene extracts, in a closed container, shake with NaOH solution. You will need to vent this often b/c pressure will build up. Discard water layer and then extract the toluene with two more portions of NaoH solution followed by a dH2O extraction. Discard all water layers.

Separate off the toluene layer, filter through a filter packed with (baked) epsom salts. Wash the epsom salts with more dry toluene. Evaporate to dryness.

Now to the dry powder, add a minimal amount of boiling absolute ethanol or isopropyl alcohol. Stirr until everything dissolves. Wrap the beaker in foil and let it slowly return to room temperature. Place the beaker in the freezer for a few hours.

Come back and you will see T-prop solid precipitated in the beaker. Filter this and wash with a few small portions of ice cold alcohol.


Any (other) chem heads? Critisism appreciated.


Andy

 

[serge]

i follow your theory, but i dont understand the logic, ok at first you are trying to remove the binders with toluene? i would use methanol, it works great. after that, im lost

 

[Andy13]

Crush pellets, stir in toluene, filter. Remove powder from filter, stir in toluene some more, filter.

The toluene will dissolve the T-prop, leaving the binders and (some of) estrogen behind

To the combined toluene extracts, in a closed container, shake with NaOH solution. You will need to vent this often b/c pressure will build up. Discard water layer and then extract the toluene with two more portions of NaoH solution followed by a dH2O extraction. Discard all water layers.
The NaOH will ionize the OH on the estradiol that was pulled in with the T-prop in the toluene extracts

Separate off the toluene layer, filter through a filter packed with (baked) epsom salts. Wash the epsom salts with more dry toluene. Evaporate to dryness.
"Drying" the non-polar layer by filtering through epsom salts removes entrained water

Now to the dry powder, add a minimal amount of boiling absolute ethanol or isopropyl alcohol. Stirr until everything dissolves. Wrap the beaker in foil and let it slowly return to room temperature. Place the beaker in the freezer for a few hours.
The is the last (crucial) purification step. Any estradiol that made it through the previous steps will be removed here since it has a higher solubility in the alcohol than t-prop. Notice- that's t-PROP. The ester has not been removed.

Come back and you will see T-prop solid precipitated in the beaker. Filter this and wash with a few small portions of ice cold alcohol.

 

[serge]

have you tried this method, or is it all just theory?

 

[Andy13]

have you tried this method, or is it all just theory?

No, I havent tried it.. And I won't have access to any of my harware until Thanksgiving.

But I'm sure as hell it's better than animals "ester removal" method.

Would you mind posting *his* method? Frankly, I can't see how this can (safely) be done without a seperatory funnel... I have all of that stuff.

 

[Nathan]

"Now to the dry powder, add a minimal amount of boiling absolute ethanol or isopropyl alcohol."

What? Isn't the bp of ethanol and/or isopropyl alcohol around room temp?

 

[serge]

Nathan, ethanol and iso propynol do not boil at RT

 

[Andy13]

"Now to the dry powder, add a minimal amount of boiling absolute ethanol or isopropyl alcohol."

What? Isn't the bp of ethanol and/or isopropyl alcohol around room temp?

Lol.. It makes you wonder how liquor stores keep their Vodka from boiling off the shelf!!

J/k Nathan... couldn't resist.. The BP's of the isopropyl alcohol is around 80deg C.

 

[serge]

A's method, he give you 2 vials #1 and #2. he wont tell you what is in each. i have not been able to determine the content of #1, i have done scans on it but did not get a perfect match.

step 1, you dissolve pellets in methanol, let the binders drop out and take the solution out

step 2, you mix solution with mixture of water and content of vial #1, let the methanol evaporate, the unesterfied test and estradiol drop out and you filter them out of the water and put the powders back in methanol

step 3, mix solution with a mixtrue of water and content of vial #2 (NaOH), evaporate methanol, filter out pure test, dry it and you got your pure test powder.

like i said, i tryed it and it worked great

 

[Nathan]

Nathan, ethanol and iso propynol do not boil at RT

Yeah, I think you're right. I think ethanol boils at about 78 degrees (Celsius). Sorry, I fucked that up.

 

[serge]

dont sweat it bro

 

[Nathan]

Hey man, I was thinking diethyl ether I guess. Doesn't that boil at room temp - about 34 degrees? I'm hurt cause I normally have a near photographic memory for numbers like universal constants, etc.

 

[serge]

diethyl ether does not boil at RT either

 

[Nathan]

diethyl ether does not boil at RT either

Dammit! I'm going to go check....diethyl ether - C4H10O - Tb = 34.7 degrees Celsius. That's pretty close to room temp. What is room temp defined to be?

 

[serge]

25C

 

[Nathan]

25C

Thanks.

 

[Andy13]

A's method, he give you 2 vials #1 and #2. he wont tell you what is in each. i have not been able to determine the content of #1, i have done scans on it but did not get a perfect match.

step 1, you dissolve pellets in methanol, let the binders drop out and take the solution out

step 2, you mix solution with mixture of water and content of vial #1, let the methanol evaporate, the unesterfied test and estradiol drop out and you filter them out of the water and put the powders back in methanol

step 3, mix solution with a mixtrue of water and content of vial #2 (NaOH), evaporate methanol, filter out pure test, dry it and you got your pure test powder.

like i said, i tryed it and it worked great

Wow.. That is shitty!! Take note that at no point in time are the esters hydrolized. You need to heat it in order to hydrolize the ester. Simply adding NaOH will not do it. If he thinks that his procedure hydrolizes the esters then that just further illustrates his ignorance on the subject of organic chemsitry.

My procedure is superior to this... But you need a seperatory funnel.

 

[cockdezl]

ANDY, at what point has your process hydrolyzed the benzoate ester off of the estradiol?

"Crush pellets, stir in toluene, filter. Remove powder from filter, stir in toluene some more, filter. To the combined toluene extracts, in a closed container, shake with NaOH solution. You will need to vent this often b/c pressure will build up. Discard water layer and then extract the toluene with two more portions of NaoH solution followed by a dH2O extraction. Discard all water layers."

In case anyone tries to do this, notice that the NaOH solution mentioned is actually NaOH dissolved in water.

 

[Andy13]

ANDY, at what point has your process hydrolyzed the benzoate ester off of the estradiol?

"Crush pellets, stir in toluene, filter. Remove powder from filter, stir in toluene some more, filter. To the combined toluene extracts, in a closed container, shake with NaOH solution. You will need to vent this often b/c pressure will build up. Discard water layer and then extract the toluene with two more portions of NaoH solution followed by a dH2O extraction. Discard all water layers."

In case anyone tries to do this, notice that the NaOH solution mentioned is actually NaOH dissolved in water.

It doesn't. It is not necessary to hydrolize this ester. It already has a free OH that will ionize.

 

[TraxZBT]

Am i gonna learn this next semester when i take organic chem??... cause if i am.. i'm about to order me some hundred packs of ritilin...

 

[Golfer18--old]

Smart mofo's

 

[Andy13]

I'm thinking of writing a "steroid chemistry" book for the aspiring kitchen chemist.

Andy

 

[serge]

if you heat up the solution the entire product is ruined, side reaction.

Andy, unlike me you have access to good chem equipment, so why dont you get a's kit and synovex-h and do the entire process and find out what exactly happens, all i know is that it works

 

[Andy13]

if you heat up the solution the entire product is ruined, side reaction.

Andy, unlike me you have access to good chem equipment, so why dont you get a's kit and synovex-h and do the entire process and find out what exactly happens, all i know is that it works

I have a decent knowledge of organic chemistry.. I don't think "A" has come up with any innovations that I have not thought of myself.

So does that mean you cannot tell me where the ester gets hydrolized?

Not being an asshole. Just being realistic.

 

[serge]

i cant tell you that, because i dont know all the ingredients in his kit, he does not tell you what they are. so what i am proposing is why dont you analize his kit and tell us what you found? i mean right now its all speculations.

 

[GaTeCrAsHeR2000]

andy, you sure you r not Professor Bunsen from the Muppets?

 

[notpuff]

i have 0 backround in chemitry coudl i still use synovex with great results