Reaktion #2307969

ord-bd2db1b60b024ea392edcc4699afbc79

Reaktionsgleichung

C=Cc1ccc(OC(C)=O)cc1
4-acetoxy styrene
ClC(Cl)Cl
chloroform
O=C(OO)c1cccc(Cl)c1
3-chloroperoxybenzoicacid
CC(=O)Oc1ccc(C2CO2)cc1
4-acetoxy styreneoxide
Ausbeute 83.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter completion of the reaction
  2. 2
    Sonstigethe 3-chlorobenzoicacid (by-product) was removed
  3. 3
    Filtrationby filtering the product
  4. 4
    Sonstigethe residual 3-chlorobenzoicacid was removed
  5. 5
    Waschenby washing 2 times with saturated sodium sulfite aqueous solution, 1 time with saturated sodium bicarbonate aqueous solution, 1 time with saturated sodium chloride aqueous solution, and 1 time with distilled water
  6. 6
    TrocknenNext, the product was dried with magnesium sulfate, and chloroform
  7. 7
    Sonstigewas removed under reduced pressure
  8. 8
    Sonstigedried for 1 day

Vorschrift

30 g of 4-acetoxy styrene and 1 L of chloroform were added into a 2 L reactor, and was stirred and cooled in iced water. 47 g of 3-chloroperoxybenzoicacid were added into the cooled solution, and the reaction was carried out at room temperature for 24 hours. After completion of the reaction, the 3-chlorobenzoicacid (by-product) was removed by filtering the product, and then the residual 3-chlorobenzoicacid was removed by washing 2 times with saturated sodium sulfite aqueous solution, 1 time with saturated sodium bicarbonate aqueous solution, 1 time with saturated sodium chloride aqueous solution, and 1 time with distilled water. Next, the product was dried with magnesium sulfate, and chloroform was removed under reduced pressure, and then the product was vacuum dried for 1 day to obtain 27.6 g of the pure 4-acetoxy styreneoxide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07368219B2uspto-grants-2008_05