02.11.2012 Views

View/Open - Illinois Institute of Technology

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Method <strong>of</strong> Procedure? Sixty three grams <strong>of</strong> sodium<br />

hydroxide were dissolved in 80 cc« <strong>of</strong> water , and<br />

treated with 150 grams <strong>of</strong> phenol in an evaporating<br />

dish. The product was heated until a film <strong>of</strong> crystals<br />

began to form- The separated crystals were dissolved<br />

by the addition <strong>of</strong> more water and the concentrated<br />

sodium phenate solution was transferred to the<br />

reacting flask-<br />

Hundred cc <strong>of</strong> carbon tetrachloride were then<br />

placed in the generating flask and fuming sulfuric<br />

acid added, drop by drop thru the tap funnel to the<br />

oarbon tetrachloride kept at a boiling temperature-<br />

The phosgene thus generated was absorbed in the<br />

reacting flask-<br />

After 2^ hours three distinct layers were formed<br />

in the flask; a solid crystalline, grayisbwhite body;<br />

a yellowish brown oily liquid on top <strong>of</strong> an aquaeous<br />

solution. On a continued passage <strong>of</strong> phosgene<br />

effervescence began to take place, showing that<br />

phosgene was being passed in an excess sufficient<br />

to overcome the alkalinity <strong>of</strong> the solution:<br />

C0Cl2*-H 2 0-»-HClt COg.<br />

HC11- (C 6 H 5 ) 2 C0 3 -^ C0 2 +2C 6 H 5 CH- HgO.<br />

-14-

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