Reaktion #1755451

ord-993aa23ebf38475b88f8db338da5905d

Reaktionsgleichung

C=CC(=O)OC
methyl acrylate
CC(C)(C)c1cccc(C(C)(C)C)c1O
2,6-di-tert-butylphenol
COC(=O)CCc1cc(C(C)(C)C)c(O)c(C(C)(C)C)c1
3,5-di-tert-butyl-4-hydroxyhydrocinnamic acid, methyl ester

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto remove the water/toluene azeotrope
  2. 2
    SonstigeA white slurry was obtained
  3. 3
    Sonstige7.2 g hazy toluene was collected in the trap
  4. 4
    SonstigeThe Dean-Stark trap was removed
  5. 5
    Sonstigea cooling condenser was connected to the reactor
  6. 6
    Sonstigewas reset to 120° C
  7. 7
    SonstigeVigorous condensation
  8. 8
    TemperaturAfter three hours of heating at 120° C.

Vorschrift

The reaction was heated to 140° C. to remove the water/toluene azeotrope. A white slurry was obtained and 7.2 g hazy toluene was collected in the trap. The Dean-Stark trap was removed and a cooling condenser was connected to the reactor. The heating was reset to 120° C. Vigorous condensation was observed and 99.1 g (1.15 mol) of methyl acrylate was added over a 45-minute period. After three hours of heating at 120° C., the 2,6-di-tert-butylphenol conversion was about 98.5% complete.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07988884B2uspto-grants-2011_08