Reaktion #486804

Reaktionsgleichung

aluminium chloride

1,3-dibromobenzene

2-bromopropionyl bromide

→

expected product

Ausbeute 76.0%

2-bromo-1-(2,4-dibromophenyl)-1-propanone

Ausbeute 76.0%

Lösungsmittel

carbon disulphide

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is maintained
2. 2
   Temperaturat reflux for 8 hours
3. 3
   Sonstigethe carbon disulphide is evaporated off under vacuum
4. 4
   workup.ADDITIONthe reaction medium is poured
5. 5
   Sonstigeonto crushed ice
6. 6
   ExtraktionThe product is extracted twice with heptane
7. 7
   Sonstigedried
8. 8
   Sonstigeevaporated to dryness
9. 9
   Sonstigeis purified on a column of silica
10. 10
    workup.ADDITIONa mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent

Vorschrift

15 g of aluminium chloride are added with caution, at 0° C., to 25 g of 1,3-dibromobenzene in 250 ml of carbon disulphide, and 22.86 g of 2-bromopropionyl bromide are then run in slowly. The mixture is maintained at reflux for 8 hours, then the carbon disulphide is evaporated off under vacuum and the reaction medium is poured onto crushed ice. The product is extracted twice with heptane, dried, evaporated to dryness and then is purified on a column of silica, using a mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent, to give the expected product.

Quelle