12-22-03 01:22
No 478374
I have two questions about two methods of decarboxylation:
../rhodium /tryptop
- Decarb in diphenylether
Is it really necessary that this reaction is carried out under nitrogen(inert) atmosphere? If it does, do you have any tips for doing this when you don't have a cylinder of N2?
- Decarb in cyclohexanol with 2-Cyclohexen-1-one katalyst.
Does anyone knows a way to make this one? I searched the forum and Organic Syntheses but found nothing?
Some kind of partial dehydrogenation of cyclohexanone?
(Stranger)
12-23-03 13:46
No 478722
(Rated as: dangerous)
the cyclohexanol/cyclohexenone decarboxylation works via the cyclohexenone's ketone group inducing the formation of carbon dioxide from the COOH, and the remaining hydrogen then goes onto the carbon chain.
The diphenylether decarboxylation works simply by high temperatures, sufficient heat and the acid groups own keto-radical decarboxylates the thing by itself. This reaction has to be done with inert atmosphere because high temperatures also increase the likelihood of oxidation, resulting in broken molecules.
there are numerous other mechanisms reported here on the hive
I experimented once with amino acids extracted from pills with acetone in a sealed container (pressure pipe) raised to 250 degrees in an oven, dangerous... yes, but there did seem to be some amount of reaction occurring in the limited experiments done, perhaps adding CO2 to the atmosphere of the pipe would help here too, as would having a pipe constructed of high grade stainless steel with a pressure release valve attached to a vent tube to remove the vented acetone (in the case of excessive pressure) from the heating device and clear of the operator.
(Stranger)
12-23-03 17:45
No 478751
yes, don't try it at home kiddies, acetone, while not as explosive as hexane or butane etc, is flammable, and a domestic galvanised pipe is not neccessarily engineered to take the pressure that could develop - and filling it too high would also risk a liquid pressure buildup which would definitely cause a rupture.
(Moderator)
12-25-03 04:34
No 478969
It is absolutely suicidal to run a gas developing reaction in a closed environment without professional eqipment.
(Stranger)
12-26-03 00:56
No 479096
Ok, we won't try this one than
.But does anyone has ideas on how to make 2-Cyclohexen-1-one???
Thanks in advance.
(Chief Bee)
12-27-03 05:46
No 479283
2-Cyclohexen-1-one can be found as an impurity in technical grade cyclohexanol, so running the decarboxylation in cheap-ass refluxing old cyclohexanol will work.
Reference:
A Novel Decarboxylation of alpha-Amino Acids
M. Hashimoto
Chem. Lett., 893-896 (1986) (../rhodium /trp.de
The Hive - Clandestine Chemists Without Borders
(Stranger)
12-28-03 02:01
No 479448
Hmmm I doubt if Merck synthesis-grade will work then, but we can try..
(Hive Bee)
01-19-04 23:58
No 483494
You sound almost as if you're about to make the horiffic mistake of spending sums of money to put your name on the list as a purchaser of chemicals...
So... you need a decently-boiling ketone?
Ever hear of tansy?
Its oil is about 77% thujone. Sure, it boils kinda right-at-the-line - about 201c, if I recall correctly - but I can assure you from whatever-personal-experiences-are-lawful
BTW...
...how much did you pay for your tryptophan? Too much?
Grab 5lbs of sunflower seeds.
Make a "giant cauldron-full-of-tea"
Pour yourself a glass. Don't drink it, because excessive tryptophan intake can have severe side effects (I had no idea where I was, or whether I was masturbating... don't.) Crash out the tryptophan with about twice the liquid volume of acetone.
::shrug:: Ghetto - but it works.
Oh, btw... if tanacetum ain't in your area - sage is about 70%. Point a fuckin' search engine at 'wid for refs... NIH in origin, I think, there archived... but fuck I'm senile... so who knows. *You* check.
Peace.
Rev. Psi Locybe, insane alchemist.
(Stranger)
02-23-04 14:26
No 490663
If the tryptamine were suspeneded in a mixture of 1,2,3,4-Tetrahydronaphthalene and acetone would it still be necessary to react under a nitrogenous atmosphere?
(Newbee)
02-23-04 17:09
No 490699
What about a Barton radical decarboxylation? Form the acid chloride, react with N-hydroxypyridine-2-thione & irradiate.