Reaktion #2338019

ord-fd3f5851dc47410e8d4f4488e34a8076

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic solution was dried
  2. 2
    Filtrationfiltered
  3. 3
    workup.STIRRINGThe reaction mixture was stirred for 2.5 hours at 60° C.
  4. 4
    Temperaturcooled on an ice-bath
  5. 5
    Waschenwashed with a 10% aqueous Na2CO3 solution and brine
  6. 6
    Sonstigedried
  7. 7
    Filtrationfiltered
  8. 8
    Sonstigethe filtrate was evaporated

Vorschrift

Metachloroperbenzoic acid (0.0501 mol) was dissolved in CHCl3 (40 ml). The organic solution was dried, filtered and the filtrate was added dropwise to a solution of intermediate 1 (0.0417 mol) and 1,4-benzenediol (0.26 g) in CHCl3 (70 ml), stirred at 60° C. The reaction mixture was stirred for 2.5 hours at 60° C., then cooled on an ice-bath, washed with a 10% aqueous Na2CO3 solution and brine, dried, filtered and the filtrate was evaporated, yielding 10.42 g of 3-fluoro-6,10b-dihydro-1aH-dibenzo-[3,4:6,7]cyclohept[1,2-b]oxirene (intermediate 2)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07317115B2uspto-grants-2008_01