Reaktion #346470

Reaktionsgleichung

ferrocene

3-chloropropionyl chloride

aluminium chloride

→

chloropropionyl ferrocene

Ausbeute 89.1%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITThe reaction mixture was left
2. 2
   Sonstigeadded ice water (30 kg) and the two layers separated
3. 3
   WaschenThe aqueous layer was washed with dichloromethane
4. 4
   Waschenthe combined organic liquors were washed with water (30 l), 2% aqueous sodium bicarbonate solution (20 l) and water again (60 l)
5. 5
   SonstigeThe organic liquors were then dried
6. 6
   Einengenconcentrated

Vorschrift

A solution of ferrocene (2.63 kg, 14.2 mole) and 3-chloropropionyl chloride (1.8 kg, 15.6 moles) in dry dichloromethane (23.5 l) was cooled to -3° and treated over 1 hour with aluminium chloride (2.08 kg, 15.6 mole). The reaction mixture was left to stir for 2 hours. To this was then added ice water (30 kg) and the two layers separated. The aqueous layer was washed with dichloromethane and the combined organic liquors were washed with water (30 l), 2% aqueous sodium bicarbonate solution (20 l) and water again (60 l). The organic liquors were then dried and concentrated affording black/brown semi-solid chloropropionyl ferrocene (3.5 kg).

Quelle