Reaktion #569996

ord-0b1945abc18a43dd8acfc2dcf7fb74a6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated in a container
  2. 2
    Sonstigeprovided with a Dean-Stark
  3. 3
    Temperaturreflux condenser
  4. 4
    SonstigeGenerated water was removed
  5. 5
    TemperaturAfter the reaction mother liquor was cooled
  6. 6
    Waschenwashed with water
  7. 7
    workup.DISTILLATIONthe solvent was distilled off

Vorschrift

20 g of 4-hydroxy-4'-biphenylcarboxylic acid, 53 g of (-)2-methylbutanol, and 4 g of conc. sulfuric acid were refluxed for 20 minutes, admixed with 500 ml of benzene, and heated in a container provided with a Dean-Stark reflux condenser. Generated water was removed. After the reaction mother liquor was cooled and washed with water, the solvent was distilled off to obtain crude 4-hydroxy-4'-biphenylcarboxylic acid 2-methylbutyl ester. The product was recrystallized from benzene-heptane mixed solvent to obtain a purified product having a melting point of 115° to 116° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04576732uspto-grants-1986_03