Reaktion #2319445

ord-710d854744154d3ab61259f48f5ea990

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGStir the reaction mixture for 1 hr by which time all starting material
  2. 2
    Sonstigewill haye reacted
  3. 3
    Sonstigeto give virtually a single product
  4. 4
    SonstigeRemove the m-chlorobenzoic acid
  5. 5
    Sonstigeformed
  6. 6
    Waschenby washing chloroform solution with aqueous NaHCO3
  7. 7
    TrocknenDry the chloroform solution (Na2SO4)
  8. 8
    Sonstigeevaporate to dryness
  9. 9
    Sonstigeto provide a colorless oil
  10. 10
    workup.DISTILLATIONDistill the oil in vacuo (1 mm)
  11. 11
    Sonstigecollect fractions
  12. 12
    workup.DISTILLATIONdistilling between 65°-72°

Vorschrift

To a stirred and cooled solution (0°-5° C.) of 4-chloro-α-methylstyrene (15.2g) in chloroform (350 mL), add m-chloroperbenzoic acid (21.6 g). Stir the reaction mixture for 1 hr by which time all starting material will haye reacted to give virtually a single product. Remove the m-chlorobenzoic acid formed by washing chloroform solution with aqueous NaHCO3 followed by water (150 mL). Dry the chloroform solution (Na2SO4) and evaporate to dryness to provide a colorless oil. Distill the oil in vacuo (1 mm) and collect fractions distilling between 65°-72° to give the title compound (8.8 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04788190uspto-grants-1988_11