Reaktion #1197143

ord-6df74131f2154544be055b6046e77a2e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe mixture is stirred for a further hour
  2. 2
    Filtrationfiltered with suction
  3. 3
    WaschenThe filtrate is washed
  4. 4
    workup.STIRRINGby shaking with 1M HCl
  5. 5
    Sonstigethe phases are separated
  6. 6
    Waschenthe organic phase is washed
  7. 7
    workup.STIRRINGby shaking with 1M NaOH
  8. 8
    SonstigeAfter purification
  9. 9
    Sonstigeby chromatography and/or crystallization

Vorschrift

10.0 g of dicyclohexylcarbodiimide in 20 ml of toluene are added with water cooling to a mixture of 9.1 g of 4-trifluoromethoxybenzoic acid, 6.0 g of 4-propylphenol, 2.7 g of dimethylaminopyridine and 30 ml of toluene. The mixture is stirred for 2 hours, 1 g of oxalic acid is added, and the mixture is stirred for a further hour and filtered with suction. The filtrate is washed by shaking with 1M HCl, the phases are separated, and the organic phase is washed by shaking with 1M NaOH and worked up. After purification by chromatography and/or crystallization, 4-propylphenyl 4-(trifluoromethoxy)-benzoate having C 59° I is obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05324449uspto-grants-1994_06