Reaktion #449875

ord-597adf5c49f94914baf2d2a90bc6c291

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Sonstigesimultaneously in the course of 1 hour
  2. 2
    workup.DISTILLATIONwas distilled off
  3. 3
    workup.ADDITIONAfter the addition
  4. 4
    TemperaturThe mixture was cooled to 90° C.
  5. 5
    workup.ADDITION250 ml of water were added
  6. 6
    SonstigeAfter separation of the phases
  7. 7
    Waschenwashing with 200 ml of water, 347 g of a viscous yellow oil of the following composition (0.3% of ethyl bromocaproate, 0.5% of residual phenol and 98% of ethyl 2-(2,4-di-tert-butylphenoxy)caproate

Vorschrift

206 g (1 mol) of 2,4-di-tert-butylphenol were melted and heated to 140° C. under nitrogen. 234 g (1.03 mol) of a 30% strength NaOEt solution in EtOH and 245 g (1.1 mol) of ethyl 2-bromocaproate were metered in simultaneously in the course of 1 hour. During the addition, EtOH was distilled off. After the addition, the reaction was ended. The mixture was cooled to 90° C. and 250 ml of water were added. After separation of the phases and washing with 200 ml of water, 347 g of a viscous yellow oil of the following composition (0.3% of ethyl bromocaproate, 0.5% of residual phenol and 98% of ethyl 2-(2,4-di-tert-butylphenoxy)caproate, remained. This corresponds to a yield of 98% of theory, based on the phenol employed.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05869735uspto-grants-1999_02