Glassware to be dried for the Grignard reaction. Left to
right: drying tube, 100-mL graduated cylinder without the
plastic base, 10-mL graduated cylinder without the plastic
base, condenser, separatory funnel without the teflon
stopcock and 100-mL round bottom flask, to be placed inside
a 1-L beaker. Ref: Pavia et.al. 3rd Ed., pp 33 and 35.
Figure 6.1
Glassware inside the 1-L beaker to be dried in the
oven.
Figure 6.2
Drying tube with calcium chloride and glass wool. See
Pavia et.al. 3rd Ed, p 536.
Figure 6.3
Dry magnesium turnings (2 g) inside the dry reaction
flask set-up.
Figure 6.4
After addition of anhydrous diethyl ether (15 mL) and
bromobenzene (9 mL), the progress of the reaction is
indicated by a cloudy solution as shown. If no immediate
reaction occurs, then use a glass stirring rod to crush a
piece of magnesium inside the flask to expose a fresh
surface of the metal in the solution by first removing the
condenser.
Figure 6.5
Why is another 25 mL of anhydrous diethyl ether added once the reaction turns cloudy?
Addition of another 25 mL of anhydrous diethyl ether as
soon as the reaction turns cloudy.
Figure 6.6
Continue sirring for a total of 45 min and the solution
will turn brownish in appearance. Keep beaker of ice-water
mixture ready for cooling.
Figure 6.7
Cooling the reaction mixture containing the Grignard
reagent. This reagent must be reacted immediately with the
methyl benzoate distilled from Expt 5.
Figure 6.8