Problem Removing Ester from Component-TH (Fina)

steeledan

New member
Anyone know what happened here?

1. Put pellets in methanol and let break up and dissolve
2. Filtered #1 with coffee filter – solution is orange
3. Filtered #2 with grade 5 Whatman filter (not syringe filter)
4. Dissolved 3 tbsp NaOH in minimum amount of H2O and added to #3 – turned dark brown
5. Let #4 sit overnight
6. Added liter of water to #5
6. Filtered #6 with coffee filter and getting brown gunk in filter and dark brown solution below

I used the same exact steps on Synovex-h and got a nice white powder and bright yellow solution below. Anyone know what happened with the fina or how to fix? I haven’t tossed anything out yet.

Thanks in advance,
Steele
 
  1. A coffee filter has a pore size so big you can drive a MAC TRUCK through it.  Use Whatmann everytime or risk losing product...
  2. After properly filtering the de-esterfied product you will need to neutralize it by washing it with water.  To test for neutral pH simply use a strip and test the BOTTOM of the filter (not  the wet powder).
  3. As the pH nears neutral the brown will turn into a deep/off yellow.

Chemo
 
Chemo..how has this process been improved? I know when I did it I lost about 40% of my product. Is it just the filter issue?
 
Thanks for the info bdc :) It's starting to clear up now. if there's a next time, I'll definately get a filtering flask and buchner funnel. Probably wind up using a brake bleeding pump..... I'll post the yeild when I'm done.
 
post detailed instructions to, if you feel like explain to us how you did everything we would greatly appreciate it :)
 
a quick question to anyone that may know:

the only whatman filters i can find are ones that screw onto syringes; in fact i've got one now that i was planning to use AFTER i used a coffee filter... do they make whatman filters in similar size to a coffee filter?

here were my theoretical steps

1)dissolve the fina carts in a oil/ba/bb solution

2)let sit for a while

3)filter entire solution through a coffee filter

4)filter remaining solution through a syringe and whatman filter into my final sterile vials

now you guys are saying product is being lost when going through the coffee filters? is it getting stuck or something?
is there anything wrong with using a coffee filter in the above-mentioned method and also filtering a second time for even smaller particles? (makes it easier on the smaller whatman filter)

if coffee-filter-sized whatman filters are available; i'd like to know where :)
 
Originally posted by wardog
Chemo..how has this process been improved? I know when I did it I lost about 40% of my product. Is it just the filter issue?
Click to expand...

There have been 4 other bros try it with Whatmann filters (versus coffee filters) and their yield was in the high 90's so I am inclined to believe the method is workable and needed only quality filters.  Of course, this only goes for the saponification of the ester and would most likely clog if doing a BA/BB/oil extraction.

Chemo
 
Originally posted by Bean
a quick question to anyone that may know:

the only whatman filters i can find are ones that screw onto syringes; in fact i've got one now that i was planning to use AFTER i used a coffee filter... do they make whatman filters in similar size to a coffee filter?

here were my theoretical steps

1)dissolve the fina carts in a oil/ba/bb solution

2)let sit for a while

3)filter entire solution through a coffee filter

4)filter remaining solution through a syringe and whatman filter into my final sterile vials

now you guys are saying product is being lost when going through the coffee filters? is it getting stuck or something?
is there anything wrong with using a coffee filter in the above-mentioned method and also filtering a second time for even smaller particles? (makes it easier on the smaller whatman filter)

if coffee-filter-sized whatman filters are available; i'd like to know where :)
Click to expand...

Your method presented is solid and will work for an injectable prep.  The conversation we were having is mainly geared (no pun intended) to saponification of the ester for transdermal prep.  The difference is that for transdermal preparation the product is lost due to large pore size of the coffee filter.  On the other hand, injectable prep does not require a smaller pore diameter since you are trying to retain large cellulose (binder) molecules.

Chemo
 
Big Daddy Chemo said:


There have been 4 other bros try it with Whatmann filters (versus coffee filters) and their yield was in the high 90's so I am inclined to believe the method is workable and needed only quality filters.  Of course, this only goes for the saponification of the ester and would most likely clog if doing a BA/BB/oil extraction.

Chemo
Click to expand...

Just curious, how were you able to determine the yield of tren in the final product? The amount that went through the filter?
 
pogue said:


Just curious, how were you able to determine the yield of tren in the final product? The amount that went through the filter?
Click to expand...

I'm going do disolve it in methanol and weigh it before disolving it in pyridine and adding decanoyl chloride. How else would i know how much decanoyl chloride to add? :) I'll post the yeild of trenbolone deconate too.

Doing the synovex was 10x easier than the component TH (fina). I think i'll try synovex plus next time. I swear, there had to be 10x more binders in the fina than the synovex. And the first fina solution was orange - is that glue or methyl cellulose or something else?

The good news it it's now tan and the ph is down to 8. hopefullly it'll only need a few more washes to become white.

Filtering stuff was so much easier in organic chem with a buchner funnel....:saw:
 
Originally posted by steeledan
I'm going do disolve it in methanol and weigh it before disolving it in pyridine and adding decanoyl chloride. How else would i know how much decanoyl chloride to add? :) I'll post the yeild of trenbolone deconate too.
Click to expand...

steeledan,

In order for your method to yield tren decanoate you will first need to saponify the ester and then react the base with the acid chloride (decanoyl chloride) in pyridine.

  • Dissolve the pellets in annyhydrous alcohol and 1 M NaOH.  Allow to sit overnight with occassional stirring.  This will saponify the ester and yield the base after neutralization.
  • Wash with water and recover the neutral powder with Buchner filtration or simply allow to dry to completeness.  If trying to push off the last remaining water it may be helpful to use the oven at low temp (100 degrees F or so) for 30 minutes to 1 hour.
  • Dissolve the powder in pyridine and add the decanoyl chloride at a ratio of 10:1 M or generally in excess.
  • Extract the esterfied powder and purify by re-crystallization.

Something to keep in mind with this reaction is the low yield that will be realized due to the 17-hydroxy being sterically hindered.  Let us know how it goes...

Another method that can be used to esterfy the base is the Fischer esterification reaction that is basically alcohol (17-hydroxy) + organic acid (heptanoic acid) + acid catalyst ===> ester.  This reaction is better suited to the task since the yields are generally better but the drawback is that the acid has to be in [EXTREME] excess. General method flow:

  • Saponify the ester, extract with water, and neutralize the powder.
  • React the base with excess heptanoic acid + acid catalyst to yield the esterfied product (tren enanthate).
  • Extract with water, wash, and purify.

Chemo
 
Originally posted by pogue
Just curious, how were you able to determine the yield of tren in the final product? The amount that went through the filter?
Click to expand...

This is for determining percent yield when removing the ester from tren (NOT FOR INECTABLE PREP):

  • Convert the mass of the esterfied material into mols
    • 1 grams of tren acetate / 312.4078 g mol(^-1) = 3.2x10^-3 mol
    • 312.4078 is the molecular weight of tren acetate
  • Calculate 100% yield
    • <!--StartFragment -->270.3706 g mol(^-1) * 3.2x10^-3 mol = .865 grams
    • This is how much you'd have if you performed the experiment to perfection and got 100% yield.
    • 270.3706 is the molecular weight for tren base
  • Saponify the ester and weigh the dry material (should be tren NE).
    • *whatever* you have grams / .865 grams *100 = % YIELD
    • For example, if you performed the experiment and got .75 grams at the end it would be .75/.865*100 = 86.7% YIELD
  • % yield is a percentage of what you got divided by what you should have gotten. 

This is figured for a 1 grams starting weight of tren acetate.  If you use more for your eperiment simply increase the numbers accordingly.  For examply, if you use 4 grams as starting material the "perfect" 100% yield would be 3.46 grams (.865 x4). To simplify this for you I have attached a spreadsheet with other info.

Chemo
 

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Last edited:
I got 15.8 grams of test base from one box of snyovex. That's about 94% yeild. I filtered everything with coffee filters followed by whatman filters. The whatman's didn't get anything extra - must have good coffee filters :) I'll know the yeild of tren base later tonight.

As far as adding the deconate ester goes, from what i've read, you only need a 1:1M ratio using an accid chloride in pyridine. Reason being that the reaction is driven far to the right because the reaction produces H+ as a by product and the pyridine neutralizes it.

Using the Fischer esterification, you need to use excess ester and acid to drive the reaction to the right. One problem might be that the longer esters arn't very soluable in water and might be hard to get rid of if you use excess amounts....

I'll let everyone know how it goes.
 
It's always the lesser of two evils ;)

The acid chloride/pyridine method is very susceptable to steric hinderance (reaction is best used with primary alcohols) so an excess amount has to be used if you expect more than an 80% yield.

I agree with your assessment of the Fischer reaction but a quick "how-to" on making a homemade LC column would do the trick ;)

BTW, I wrote a general abstract for the methods Invalid Link Removed

Chemo
 
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