| Overview |
| Instructions |
| Operating scheme |
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; Side reactions |
Oxidation of anthracene to anthraquinone |
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Synthesis instructions as PDF file for printing |
ReactionIn each of the grinding cups a mixture of 3.8 g aluminum oxide, and 3.80 g (24.1 mmol) potassium permanganate is placed. 360 mg (2.02 mmol) Anthracene
and 380 mg (21.1 mmol)
water
are added to each cup and the reaction mixture is ground at 800 rpm for 10
minutes.
.
Work upThe product is isolated by flash chromatography of the reaction mixture. A frit G3 with ground joints is used as the separation column, magnesium sulfate
as the stationary phase and
dichloromethane
as eluting solvent. The frit is filled with a 2 cm layer of magnesium sulfate
and then to the upper edge of the magnesium sulfate layer with dichloromethane.
A 100 mL round-bottom flask serves as collecting flask.
The red-brown solid from the grinding cups is transferred onto the magnesium
sulfate layer using a powder funnel. One grinding cup with the grinding balls
is washed thoroughly with 10 mL dicholoromethane which is also then used to
wash the second grinding cup. The liquid is then poured onto the packed column.
The ground glass adaptor which can be connected via tubing to the air or
nitrogen line is placed onto the frit and the liquid phase under slight
pressure (1.1 - 1.2 bar)
.
is passed over the column until no further liquid is present above the solid
phase. One refills the frit with 10 mL dichloromethane and and elutes, again
under slight pressure, a further two times. Thereafter the column is allowed to
run dry. The solvent is evaporated completely from the eluted solution using
the rotary evaporator.
Anthrachinone
remains as a yellow solid.
Yield: 420 mg; melting point 248-287 °C; Purity according to GC: > 99% Duration of the experiment1 hourWhere can I stop the experiment?The ground mixture is stable at room temperatureRecyclingThe evaporated dichloromethane is collected and redistilled |
Suggestions for waste disposal |
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