Reaktion #652009

Reaktionsgleichung

(4-Chlorophenyl)(4-nitrophenyl)methanone

p-Toluene-sulfonic acid

Toluene

water

→

2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane

Ausbeute 91.0%

Lösungsmittel

Ethylene glycol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 48 hours
2. 2
   SonstigeThe solvent was evaporated
3. 3
   workup.DISSOLUTIONThe residue was dissolved into ethyl acetate (5 l)
4. 4
   Waschenwashed twice with a K2CO3 10% solution
5. 5
   SonstigeThe organic layer was separated
6. 6
   Trocknendried (MgSO4)
7. 7
   Filtrationfiltered
8. 8
   Sonstigethe solvent was evaporated
9. 9
   workup.STIRRINGThe residue was stirred in DIPE
10. 10
    Filtrationfiltered off
11. 11
    Sonstigedried (vacuum, 40° C., 24 hours)

Vorschrift

Toluene (1900 ml) was stirred in a round-bottom flask (51) using a water separator. (4-Chlorophenyl)(4-nitrophenyl)methanone (250 g) was added portionwise. p-Toluene-sulfonic acid (54.5 g) was added portionwise. Ethylene glycol (237.5 g) was poured out into the mixture. The mixture was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was dissolved into ethyl acetate (5 l) and washed twice with a K2CO3 10% solution. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried (vacuum, 40° C., 24 hours), yielding 265 g (91%) of 2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane (interm. 5-a).

Quelle