Place a spinvane and 0.05 g of magnesium turnings into an oven-dried 5-nth conical vial….
Place a spinvane and 0.05 g of magnesium turnings into an oven-dried 5-nth conical vial. 2. Attach the Claisen adapter to the conical vial. On the curved joint, attach a drying tube filled with calcium chloride. Place a Teflon-rubber septum and screw cap on the straight portion of the adapter. Clamp the appa-ratus so that it sits centered on a heater-stirrer (no stirring at first and NO HEATING). 3. Measure 4 nth of anhydrous diethyl ether in a second 5-mL conical vial and cap it. You should use this diethyl ether to make the solutions needed throughout this experiment 4. Weigh a 3-mL conical vial and dispense 0.35 mL of bromobenzene into the vial. Reweigh the vial to deter-mine the weight of the bromobenzene and record this in your lab notebook. 5. Add 1.0 mL of diethyl ether to the vial containing the bromobenzene. Using your syringe, add 0.40 mL of this solution to the reaction apparatus through the Teflon septum. At this point of the reaction you should observe the evolution of bubbles and/or the solution should become cloudy or pale yellow indicating the reaction has started. If the reaction does not start, remove the rubber septum from the apparatus and insert a microspatula and twist it so as to crush the magnesium against the glass surface. This should break some magnesium pieces and start the reaction. 6. Add the remaining solution of bromobenzene from the syringe slowly over a period of 5 min. Rinse the ini-tial vial containing bromobenzene with 0.5 mL of diethyl ether and transfer to the reaction vessel (this assists in achieving quantitative transfer of the bromobenzene). The reaction mixture should stir for an additional 15 min.
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