1.08 g (1.09 mL, 10.0 mmol)
anisole,
1.53 g (1.42 mL, 15.0 mmol)
acetic anhydride
and 0.288 g
Zeolite H-BEA 25
are placed into a 10 ml round bottom flask containing a magnetic stir bar and
fitted with a reflux condenser. The reaction mixture is heated with stirring
for 6 hours to 150 °C.
Work up
The catalyst is filtered off using a Buechner funnel (Ø = 2.0 cm) and washed with 15 ml
ethanol.
The filtrate is concentrated on a rotary evaporator.
Crude product yield: 1.35 g;
The crude product is distilled in a kugelrohr distillation apparatus at 25 hPa
(oil bath temperature up to 165 °C).
Yield: 1.11 g; melting point 35.6-37.5 °C;
white solid
Duration of the experiment
6 hours for the reaction, 1.5 hours for the distillation
Where can I stop the experiment?
After heating under reflux and after concentrating with the rotary evaporator.
Suggestions for waste disposal
Waste
Disposal
distillation residues (dissolve in a small amount of acetone)