تفاعل #2307969

ord-bd2db1b60b024ea392edcc4699afbc79

معادلة التفاعل

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
المردود 83.7%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter completion of the reaction
  2. 2
    أخرىthe 3-chlorobenzoicacid (by-product) was removed
  3. 3
    ترشيحby filtering the product
  4. 4
    أخرىthe residual 3-chlorobenzoicacid was removed
  5. 5
    غسيلby 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
    تجفيفNext, the product was dried with magnesium sulfate, and chloroform
  7. 7
    أخرىwas removed under reduced pressure
  8. 8
    أخرىdried for 1 day

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07368219B2uspto-grants-2008_05