Organic 2 Review Problem 177

Organic 2 Review Problem 177 - P REPARATIONS 1 61 This...

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PREPARATIONS 161 This preparation must be performed in a fume-cupboard, because nitrous fumes are evolved during the nitration. A ground-glass flask and air condenser (Fig. 22(A) and (c), p. 43) should preferably be used. Place 15 ml. of fuming nitric acid (a 1 , 1-5) in a 150 ml. flask and add carefully with shaking 20 ml. (37 g.) of concentrated sul- phuric acid and then some fragments of unglazed porcelain. Fit a reflux air-condenser securely to the flask, and then add slowly down the condenser 12 ml. (14-5 g.) of nitrobenzene: do not add more than 3 ml. of the nitrobenzene at a time, and after each addition shake the flask to ensure thorough mixing of the contents. Now heat the flask on a boiling water-bath for i hour, both the flask and the condenser being securely clamped in position if joined by a cork, which the acid fumes evolved may attack and weaken. Shake the flask vigorously from time to time throughout this period of heating. Finally pour the mixture carefully with stirring into an excess of cold water (about 300 ml.), whereupon
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This note was uploaded on 09/19/2011 for the course CHM 2211 taught by Professor Castalleano during the Fall '06 term at University of Florida.

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