WITH THIONYL CHLORIDE 137 i flask is protected from moisture by a calcium chloride tube which is removed only during the addition of reagents. Heat and hydrogen chloride are evolved during the vigorous reaction, and after standing at room temperature for an hour nearly all the acid and phosphorus pen-tachloride are in solution. The mixture is warmed on the steam bath for about five minutes, in order to ensure complete reaction, and then is chilled until the benzene shows signs of beginning to solidify. At this point a solution of 80 cc. (about 0.7 mole) of anhydrous stannic chloride in 80 cc. of dry thiophene-free benzene is added rapidly with swirling or mechanical stirring, whereupon an orange-yellow complex separates. After standing for fifteen minutes in ice water the mixture is hydrolyzed by the addition of ice followed by 250 cc. of concentrated hydrochloric acid. A small amount of ether (about 25 cc.) is added to hasten the hydrolysis of the stannic chloride addition complex (which is soluble in
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This note was uploaded on 11/20/2011 for the course CHM 2210 taught by Professor Reynolds during the Fall '01 term at University of Florida.