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Synth for sodium ethyl sulfate?
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thenewrunne
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Synth for sodium ethyl sulfate?

 Thu Apr 21, 2005 7:03 am		 Reply with quote
So far I haven't seen a synth for this yet, I saw this one for diethyl sulfate on Rhodium's archive.
Quote:

Preparation of Diethyl Sulfate
Procedure

Ninety grams of sodium sulfate is placed in a dry 1 liter flask connected with a condenser and a receiver arranged for vacuum distillation. The flask is heated by means of an oil bath to 155-165°C. The apparatus is exhausted as nearly as possible by means of a filter pump, and misture of 50 grams of ethanol and 104.5 grams of concentrated sulfuric acid is allowed to drop through a capillary tube on the sodium sulfate at a rate of 120-150 drops per minute. The distillation of the mixture requires about one and one half hours for completion. The distillate, which consists of ethanol and diethyl sulfate is poured into a separatory funnel, the ethanol may be recovered for further use. The diethyl sulfate is washed with a dilute solution of sodium carbonate and then several times with cold water, then dried with anhydrous sodium sulfate, yielding 32.4 grams.

Reference: JACS 46, 999-1001 (1924)


This can be using in the synth for nitroethane, yes?

Would it be OK to use 35% H2SO4, or is concentrated 98%+ needed?

Are there other synths for sodium ethyl sulfate out there that are as good as this?
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thenewrunne
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 Thu Apr 21, 2005 7:09 am		 Reply with quote
Embarassed Sorry. I just found the other post with the title:

Quote:

A condensation from the late Rhodium's Nitroalkane FAQ:

Materials
23g CaCO3, finely powdered
16mL conc. H2SO4(aq)
40mL EtOH
200mL H2O
suff. sat. Na2CO3(aq) to basify
suff. CaCl2 to dessicate

Procedure

1. Slowly add 16mL H2SO4(aq) to 40mL EtOH.
2. Heat to a gentle boil for 45 minutes, then let cool.
3. Pour solution into 200mL H2O.
4. While stirring vigorously, add 23g CaCO3 to solution.
5. Heat solution to 60°C and, while hot, collect product via suction filtration, discarding solids.
6. Basify filtrate with Na2CO3(aq) dropwise.
7. Evaporate filtrate on a water bath to saturation and let stand overnight.
8. Collect product via suction filtration, discarding solids.
9. Dry in a dessicator with CaCl2.


Yield: 12g sodium ethyl sulfate


Is there any benefit of using sodium ethyl sulfate vs. diethyl sulfate to make nitroethane?

(sorry for the double post)
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icecool
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 Sat Apr 23, 2005 5:49 pm		 Reply with quote
Why is suction filtration needed the crystals aren't the product so it can be filtrated by gravity right?
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IndoleAmine
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 Sat Apr 23, 2005 9:41 pm		 Reply with quote
suction is faster + more efficient than gravity filtration.
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