Swim recently tried to preform the kolbe electrolysis of 5-HTP in methanol w/ excess acetic acid (total solution <4% water). Sadly, it did not work
. Here is a more detailed overview:
Reagents/Apparatus:
- 5 pills of 5-Hydroxytryptophan (50mg 5-HTP/pill, the packaging
excess is "white rice powder") Purchased from NOW-foods ltd.
- 15 mL 33% HCL (Muriatic acid)
- 40 mL of saturated Sodium Acetate in 99.95% reagent grade Methanol
- 210 mL 99.95% methanol ("Heet" methyl alcohol from a hardware store
I called the company, it should be of that purity)
- 300 mL Ethyl Ether+Heptane (starter fluid)
- Excess of Sodium Bicarbonate (arm and hammer baking soda)
- 2 pure Ag electrode (5cmx1cmx.33cm purchased at a jewlery store)
- 12V 1 Amp battery charger
Experimental:
So swim hooked the electodes up and placed everything (except the
ether and baking soda) into a 500mL beaker and let run for ~32 hours,
keeping the solution in a room temperature (20-25 degrees) and in an
ice-bath while swim was not present (~12 hours). At T=O the solution was
clear, but after about 24 hours it started to turn yellow and after 32
hours the solution was burnt yellow in colour. So, swim basified the
solution and it turned deep forest green. The solution was then
poured into a sep funnel with the ether, seperated only once, due to
swim's limited amount of ether (yeah, yeah, swim knows, swim'll get to the
hardware store soon....).
Now, when swim added more acid to the ether, a precipitate should form,
but it does not. So swim filtered the green solution and was left with a
filtrate of white rice power, mixed with a brown substance swim could not
identify and a green supernatant.
So, after swim rigorously tested the eventual powers to form from the evapourated methanol (5-HO-t should be pretty soluable in methanol, likw 5-HO-indole, which is incredibly so)..... Anyway, what went wrong? Swim folled the procedure he found on a german website he has since lost, a procedure for the kolbe electrolysis and generation of butane, help swim, please.