Réaction #56392

ord-b1d0998d3cf545b793e561524dc0c9a6

Conditions de réaction

Température
20°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe mixture is heated
  2. 2
    Températureunder reflux for 20 hours
  3. 3
    Températureto cool
  4. 4
    AutreThe white precipitate obtained
  5. 5
    Filtrationis filtered off
  6. 6
    Concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C
  7. 7
    AutreThe oil thus obtained
  8. 8
    Lavagewashed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time)
  9. 9
    SéchageThe ethereal phase is then dried over anhydrous sodium sulphate
  10. 10
    Filtrationfiltered
  11. 11
    Concentrationconcentrated to dryness under reduced pressure (20 mmHg) at 40° C

Mode opératoire

Sodium (5.7 g) is dissolved in ethanol (160 cc), and a solution of para-cresol (27 g) in ethanol (20 cc) is added. The mixture is stirred for 1 hour at 20° C. and ethyl dichloroacetate (20 g) in solution in ethanol (20 cc) is then added. The mixture is heated under reflux for 20 hours and then allowed to cool. The white precipitate obtained is filtered off and the filtrate is concentrated to dryness under reduced pressure (20 mmHg) at 40° C. The oil thus obtained is taken up in diethyl ether (300 cc) and washed twice with N sodium hydroxide solution (100 cc each time) and twice with distilled water (100 cc each time). The ethereal phase is then dried over anhydrous sodium sulphate, filtered, and concentrated to dryness under reduced pressure (20 mmHg) at 40° C. Ethyl 2,2-bis(4-methylphenoxy)acetate (29 g) is thus obtained as a yellow oil.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04225589uspto-grants-1980_09