08-14-03 02:44
No 453438
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.
(Hive Addict)
08-14-03 04:07
No 453448
Just curious, what exactly are you trying to produce? I could only find references to the Kolbe reaction being used to convert phenylalanine into meth.
Also, Post 75904 (jim: "Re: Kolbe synth", Chemistry Discourse) claims that you cannot use silver electrodes. Nobody confirmed or denied this claim, but it might be worth looking into. ../rhodium /electro
I have little to no experience in chemistry (much less the Kolbe reaction), I'm just trying to learn about a thing that is entirely foreign to me by attempting to help others. So if I have said something completely retarded, or this post is of no help whatsoever, that is why.
(Stranger)
08-15-03 07:42
No 453667
If it's any help, and you can read german, here is the basic procedure swim followed: http://www.ph-weingarten.de/homepage/fae
And, while swim doesn't have the lit source available, swim has read before that the electrode material isn't terribly important (obviously Pt is better than Ag, but what'cha gonna do? Even that may not be true, since the anode really doens't react or do anything in the reaction, I imagine it could be anything [I've seen it be crazy stuff like diamond or Mo in some other places, I think...] One must consider the pocketbook). Personally, I think his mistake was that the intermediate wasn't able to be substituted with an electron withdrawing group (such as I, from PI3 perhaps.....). The colour change seems to indicate that an indicator was formed, and just by glancing at other indicators, many seem to involve an aromatic alcohol (present) as well as some other area of unsaturation/pushable electrons conjugated with the aromatic compound (which would be present if an alkene were formed, rather than an alpha-methyl group).
As to what swim is trying to make, well, A,N,N,O-tetramethylserotonin seems like it could be interesting, no? But should this process prove viable there is no reason why AMT and amphetamine couldn't also be readily synthesized by this method. Ultimately though, it's just playing with chemicals, no intent of injestion, just playing a little god.
(Hive Bee)
05-11-04 02:13
No 506325
ho did you clean out the white rice powder? i have been trying something similar but have been having problems with the rice powder maybe you had the same problem?
(Hive Addict)
09-23-04 00:44
No 532804
Swim has been following this thread Post 459300 (tpower9s2003: "DL-Phenylalanine--->PEA--->Dl-amp
So one would pretty much want to substitute the muriatic with GAA, the 5-HTP with "cleaned" phenylalanine and the silver with platinum.
Swim found a company that makes "pure platinum" spark plugs. The electrode is platinum and the threads are nickle plated. Would these work as an OTC source?
This produces d-amphetamine and not meth?
Refuse/Resist