Antibody decided to have a dream of using Toennies method of producing pseudonitrosites in using GAA as a solvent. It was likely a successful dream but being unfamiliar with nitropropenes cannot say for certain.
After expereiencing a particularily fierce mind explosion antibopdy was cast into a deep coma, and had this dream.
20ml asarone was added to 200ml GAA, asarone takes a couple of moments to go into solution. Meanwhile a 100ml of saturated aqueous NaNO2 solution is prepared.
With no stirring or cooling the NaNO2 solution is dripped into the Asarone/GAA over the course of three hours. Each drop of NaNO2 solution seemed to produce an initial precipitate that is almost immediately disolved.
At the end of addition a viscous bright yellow layer begins to appear on top. antibody initially thought that this was simply the asarone being forced out of solution by the Aqueous NaNO2, however this layer was considerably brighter than the asarone which had only the faintest traces of light yellow to it. So maybe it is a layer of monomer forming (maybe was greenish but antibody is colour blind so cannot say for certain)
It was left overnight and in the morning the yellow layer was even larger. so the entire rxn was tossed into a sep funnel and left to separate. That evening antibody goes back, and the entire solution has turned BRIGHT PURPLE! two phase cloudy light purple on bottom, and the top layer is deep bluberry, and is so viscous that it clogs the sep funnel. It is partially crystalized. This seems promising.
200ml of 8% KOH in ethanol is added to sep funnel and shaken alot. It goes into solution mostly still some solids at bottom, so heavy mag stirring is attempted to bust them up.
This results in the stuff that had been in solution all of a sudden sticking togather in an yellowish white blob of gum. This is hell to break up. Try crushing with spoon and with herculean manual shaking. Finally most of it busts up. and solution is very cloudy and dirty yellow/orange with just a couple gobs of gum on bottom.
This is chilled in freezer for half hour (no ice) then mixed in a big erlynmeyer flask with 1l of 3n HCl, initially there is alot of off white/yellowish precipitate that fell out, but after heavy shaking all the precipitate floated to the top, it is bucknered and washed with water and dilute HCL, then left to air dry,
After is is dry the crystals are weighed 16.4g they are very crunchy with the majority being yellowish off white kinda colour, but the chunks of gum that never broke up when those are crushed there is Bright orange crytals inside, much more crystaline than the rest, they comprise maybe 15% of the total.
Antibody is not sure what he has is in fact nitropropene, any opinions?
Antibody is not sure if sodium acetate was produced and crystallized and what would happen to it when placed in the alkaline alcohlic solution, or if potassium hyponitrite was produced. Antibody thinks one or the other of the crystals is nitropropene. and the rest is something out.
Antibody has been dreaming these pseudonitrosites for awhile now, and would greatly appreciate the opinion of a more enlightened dream interpreter the himself.
antibody thinks he has given a pretty detailed account and hopes it will be eneough for some bee to tell em if heis dreaming in the right direction.
Found the purple colour very perplexing, any thought on that? it disappeared immediately on going into KOH solution?
Jimi loves ya!