All u Chem wizards - I need help on test ester

Lets say I (or someone like me) had access to some Test base (TNE) and wanted to make Test Prop out of it via fisher esterification and then refine it a bit. Also lets say I (or someone like me) had access to good lab equipment like buchi rotorvaps, heater/stirrers, condensers and such - so no need to describe it via kitchenware - does anyone know how to go about this to get the highest yeilds (dont want to waste my powder)?

1) Now I understand that TNE has a mol wt of 288 and propionic acid has a mol wt of 74. So to get equimolar amts do I add a 74:288 ratio of grams of test/prop? Why then does the finished TP have a mol wt of 344??? Oviously something is lost in the reaction - oooooohhhhh - water (mol wt of 18)..... ok..... but is that right about the ratio? about 4 grams of prop for every gram of test?

2) what is best catalyst? sulfuric acid? how do I isolate it and get the water out and the catalyst? salt?

3) how do I purify it without losing much?

4) what equip do I need and how do I set up the glassware for the process described?

Much thanks!

Cycleon,

That's a tough one I'd say your best bet is to contact Billy Bathgate. I'm sure he'll be able to help you out. IMO he's the one of the best as far as questions like this go.

xxxl83

CHEMISTRY CLASS!!!!!!!!!!! RUNNNNN!!!!

ahhh but this is applied chemistry - much more fun and gratifying :D

I will give you a bump and also recommend Billy Bath for the issue. And applied chem is the best, wish they had FINA 101 in college. ahahahaa

Pain

bump for Billy

bump for Billy

bump

cotact billy or superchicken

You can't do it @ home....without proper safety....propionic acid is
very caustic and will burn everything it touches. You need a mask to
deal with it. Test prop costs the same as TNE so why fucking bother?

I have gotten my answers - but thats to all for your help!

sorry, I was moving and jsut now got your PM

I could have answered them all though lol

1) Id go with about ~2.5:1 molar ratio so 10 grams per gram test

2) Sulfuric is what I would use, or reagent grade HCL, but you dont need much really. At the very end, you want to neutralize everything with a tertiary base like tert-butoxide or something.

3) column chromotography would work great, but after you neutralize everything, and get all your product out, a recrystalization would work well. if in doubt ever, do a TLC on it or GCMS

4) Id say start with a stir/hot plate, 1000ml beaker, youll need some solvent, like say acetone, youll want a good filter, then if you want to do a column, you need it and the silica gel, thats about it really..you could use a smaller beaker to do your recrystallizations is


You could also go the acid-choloride route..which youll need about all the same except youll need some pyradine.


dont blow shit up

Damn Billy I was waiting to see when you were gonna get over here to answer this. I was ready to goto bb4life to track you down.

Anyway I knew you were the man for this question.

xxxl83