chucknorris
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What just happened..? Ethyl Sulfate attempt..
So I attempted to vacuum distill ethyl sulfate freebase. At the beginning some white fumes appeared which aspirator sucked off, and then some clear
liquid distilled over. But then, the yellow-brown ethyl sulfate solution at the reaction flask turned eventually into black goo, the sugar-sulfuric
acid - like stuff you all know from school. I tried to wash it off with water when it cooled, but it only partially dissolved and black bits were left
all over. I had no gas mask on at the beginning, and I coughed some very irritating fumes and left the flask immediately and came back with mask on.
Could in this process, when the vacuum was 32mbar and temperature up to 120 celsius, produce some highly toxic substances that could cause harm by
single inhalation? Chemicals involved are/were sodium bisulfate and denatured ethanol. Some possible hazards that I can find out COULD be diethyl
sulfate and hydrogen sulfide, latter being just a thought, and in no time i could smell any sort of "rotten egg", and since I work in oil industry, I
know very well what that stuff smells like. An hour has gone and I feel little dizzy, but I am not highly concerned, because I slept only 1 hour last
night. 
[Edited on 20-7-2012 by chucknorris]
[Edited on 20-7-2012 by chucknorris]
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zoombafu
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Did you synthesize it with sulfuric acid and ethanol? If it decomposed it would go into ethylene and sulfuric acid I believe.
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chemrox
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"ethyl sulfate freebase" is not a known substance. Freebases are generally amines that are "freebase" by not being associated with an acid such as
HCl or oxalic acid. To clean your flask try soaking it with 20% NaOH solution for a few minutes and then get to work with a soft brush. Did you look
up a synth for ethyl sulfate? As I recall it requires careful temperature control or you end up with diethyl ether or ethylene. Either one could
ignite and cause some real grief.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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chucknorris
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I have synthetised nearly a kilo of (sodium) ethyl sulfate so far with good success. You can find my description at the topic which is about this
substance. With freebase I mean the liquid oily form of ethyl sulfate which turns into white powder when baking soda is administered. This was just a
test were it possible to purify the ethyl sulfate oil into clear 99.9% liquid, but obviously there are certain challenges.
As said, I used sodium bisulfate and denatured ethanol.
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