반응 #346470

반응 방정식

ferrocene

3-chloropropionyl chloride

aluminium chloride

→

chloropropionyl ferrocene

수율 89.1%

용매

dichloromethane

반응 조건

후처리

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

실험 절차

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).

출처