Reaktion #1844072

ord-fe65d43e86444eecaf8d708634fbde03

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe hydrolysis reaction
  2. 2
    SonstigeAfter completion of the reaction
  3. 3
    workup.ADDITIONwas added
  4. 4
    Extraktionfollowed by extraction
  5. 5
    SonstigeThe water layer was separated with a separatory funnel
  6. 6
    Waschenthe toluene layer was washed with water (317.9 g)
  7. 7
    EinengenThen, the toluene layer was concentrated by distillation under ordinary pressure for the removal of toluene, which

Vorschrift

The above ethyl 2-(2,4-di-t-amylphenoxy)butyrate (317.9 g) and 27% aqueous sodium hydroxide (401.4 g) were placed in a 3-liter flask. The mixture was kept at 98° C. for 6 hours, and the hydrolysis reaction was completed. After completion of the reaction, the mixture was adjusted to pH 2 or lower by the addition of 40% aqueous sulfuric acid (349.9 g) and water (250 g), and toluene (317.9 g) was added thereto, followed by extraction. The water layer was separated with a separatory funnel, and the toluene layer was washed with water (317.9 g). Then, the toluene layer was concentrated by distillation under ordinary pressure for the removal of toluene, which afforded a concentrated solution (357.6 g) of the carboxylic acid compound in toluene. The analysis revealed that the concentrated solution contained the desired carboxylic acid compound in a yield of 99% on the basis of the raw material ester compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05442114uspto-grants-1995_08