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Author: Subject: Nitroethane from ethylsulfate, Desseigne variation.
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[*] posted on 24-9-2020 at 09:26

Curious in making the ethyl sulfate from ethanol and sodium sulfate. Tried this not long ago, but my setup was all wrong.
I like Chuck Norris' approach on page two and that is what I followed.

500ml 3 neck RBF. Center neck has a mechanical stirrer and an addition funnel attached using a Claisen adapter.
one side has a thermometer, the other side has a reflux.

Put in 150g of pool sodium bisulfate. Into the addition funnel was placed 150g 95% ethanol.
The sodium sulfate melts at low temps, so it is warmed on mantle until it liquifies.
As soon as the ethanol drip is started, it reacts, very exothermic.

My problem last time was the ethanol was dripped from one of the side necks, which cause the salt formed to stick to side of flask.
This time, I will drop from center of flask in hopes to prevent the formed salts from sticking to side of flask.

My understanding is once the ethanol is added, I should gently reflux for 30 minutes.
Place the flask in the freezer to bring to 0C, then filter off ethyl sulfuric acid and any unreacted ethanol.

The ethanol will be removed via rotovap, leaving the ethyl hydrogen sulfate behind.
This sound about right?
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