반응 #2307969

ord-bd2db1b60b024ea392edcc4699afbc79

반응 방정식

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
수율 83.7%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After completion of the reaction
  2. 2
    기타the 3-chlorobenzoicacid (by-product) was removed
  3. 3
    여과by filtering the product
  4. 4
    기타the residual 3-chlorobenzoicacid was removed
  5. 5
    세척by 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
    건조Next, the product was dried with magnesium sulfate, and chloroform
  7. 7
    기타was removed under reduced pressure
  8. 8
    기타dried for 1 day

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07368219B2uspto-grants-2008_05