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21st February 2012 @ 20:58
PS = Pictet-Spengler

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This experiment has been put on hold. No further work performed as of 24/02/12.
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START: 23/02/12
FINISH:

Background

Scheme%20KAB16-1.png


Hazard and Risk Assessment
Hazard and Risk Assessment KAB16-1


Previous Related Experiments
Preparation of Imidobis(sulfuryl chloride) (KAB15-1)

Following Experiments


Procedure

23/02/12 - Saturation of diethyl ether with gaseous HCl
Neat sulfuric acid in a pressure equalising dropping funnel was added dropwise in portions to a 3-necked round bottom flask containing sodium chloride. The generated hydrogen chloride gas was sparged through diethyl ether (1 L) at -78 °C. The sodium chloride flask required changing after excessive formation of sodium bisulfate.
Saturation of ether setup
Saturation of ether setup (annotated)



Summary and Conclusion


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NOTES 23/02/12
- After about half of the H2SO4 was added, the NaOH solution backflowed into the ether solution. The process was terminated and while the ice was still frozen in the ether solution, the acidic ether was canulated into an oven-dried 1 L pyrex jar. The ether will require further acidification before use in the column.
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Linked Posts
Attached Files
Scheme KAB16-1
Hazard and Risk Assessment KAB16-1
Saturation of ether setup
Saturation of ether setup (annotated)
Ice in ether