Reaktion #2318792

Reaktionsgleichung

2-chloro-4-[(p-heptylbenzoyl)oxy]benzaldehyde

Jones' reagent

→

2-chloro-4-[(p-heptylbenzoyl)oxy]benzoic acid

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONWithin 40 minutes there are added dropwise
2. 2
   Sonstigeprecipitated inorganic material
3. 3
   Filtrationis then filtered off under suction
4. 4
   workup.ADDITIONthe filtrate is diluted with 300 ml of water (the product
5. 5
   Sonstigeprecipitating),
6. 6
   Einengenconcentrated on a rotary evaporator to about 300 ml
7. 7
   Sonstigethe suspension obtained in suction
8. 8
   Filtrationfiltered
9. 9
   FiltrationThe suction filter material
10. 10
    Waschenis washed three times with 50 ml of 10% aqueous acetone
11. 11
    Sonstigedried
12. 12
    Sonstigerecrystallized from about 60 ml of benzene

Vorschrift

The resulting, crude 2-chloro-4-[(p-heptylbenzoyl)oxy]benzaldehyde is dissolved in 350 ml of acetone. Within 40 minutes there are added dropwise thereto 30 ml of Jones' reagent, the mixture warming slightly. The mixture is stirred for a further 1 hour, precipitated inorganic material is then filtered off under suction, the filtrate is diluted with 300 ml of water (the product precipitating), concentrated on a rotary evaporator to about 300 ml and the suspension obtained in suction filtered. The suction filter material is washed three times with 50 ml of 10% aqueous acetone, dried and recrystallized from about 60 ml of benzene. There are obtained 13.8 g of 2-chloro-4-[(p-heptylbenzoyl)oxy]benzoic acid, m.p. 108° C. (nematic).

Quelle